Trimethylsilylcyanide

1. Then 982.6 mg (9.9 mmol) trimethylsilylcyanide is added dropwise and stirred at RT for 48 h. (Web site)
2. Trimethylsilylcyanide (267 ul, 2.0 mmol) was added to the solution and the resultant mixture was stirred for 48 hours. (Web site)

Dry Thf

1. Dry THF (200 mL) is added followed by dry pyridine (5.54 g, 70.1 mmol). (Web site)

Additional

1. After completion of the reaction, 10 mmol of 2-bromo-1,1-diethoxyethane was added and the reaction was continued for an additional 2 days. (Web site)

Calcium

1. Although calcium flow to and from the bone is neutral, about 5 mmol is turned over a day. (Web site)

Hour

1. Ia was prepared from 0.70 g (2.7 mmol) of triphenylphosphine and 0.53 g (2.7 mmol) of α-bromoacetophenone by ball-milling for one hour under helium.

Yield

1. Yield: 22.7 g (55.2 mmol, 92%). (Web site)

Cooling

1. To the solution was added 500 ml dry tetrahydrofuran and, after cooling to -20 DEG, 4.0 g (35.8 mmol) of freshly sublimed potassium-t-butoxide was added.

Nitrogen

1. Methyl 2,4-dihydroxybenzoate (5.1 g, 30.33 mmol) and triphenylphosphine (9.52 g, 36.3 mmol) were stirred in THF (200 ml) under nitrogen.

Ethanol

1. The nitroamine (1 mmol) obtained as above is dissolved in ethanol (10 mL) and treated with tin (II) chloride dihydrate (5 mmol). (Web site)

Solvent

1. The aqueous phase is extracted four times with the given solvent (when alkylating 40 mmol, about 20 ml).

Aqueous

1. Combine 0.70 g (1.4 mmol) of the product of Step D and 8 mL of concentrated HCl (aqueous) and heat the mixture at reflux overnight. (Web site)

Lipase

1. As a rule, 1000 units of lipase are added per mmol of heteroatom-substituted amine. (Web site)

Polymerization

1. The procedure of Example 1 was repeated except that in the polymerization of ethylene in (2) the amount of indene used was changed from 5 mmol to 1 mmol. (Web site)

Equiv

1. Tetrabutylammonium fluoride (2.0 mmol, 2.0 equiv) was dissolved in dry THF (2 mL) at room temperature under an atmosphere of dry nitrogen. (Web site)

Sodium Methoxide

1. The reaction mixture was cooled in ice-water and sodium methoxide (2.70 g; 50 mmol; 2 equiv) was added. (Web site)

Colorless Oil

1. C. to obtain 5.0 g (14.7 mmol) of methyl 3-octyl-tridecanoate as a colorless oil. (Web site)

Methylene Chloride

1. Ten millimoles (mmol) of the diene and 5 mmol of the dienophile were dissolved in about 25-50 milliliters (ml) of methylene chloride. (Web site)

Tetrahydrofuran

1. Tetrahydrofuran (30 ml) was added, followed by 3M sodium hydroxide (10 ml, 30 mmol) and 30% hydrogen peroxide (10 ml, 100 mmol). (Web site)

Methyl Iodide

1. The reaction mixture was refluxed for 2.5 h after which it was cooled to -10 DEG to 75.mu.l (1.2 mmol) methyl iodide was added.

Methanol

1. Methanol (40 mL) and aqueous sodium hydroxide (8.2 g of a 50% solution, 102.5 mmol) were added to the mixture.
2. A solution of 3-bromo-2-oxo-propionic acid ethyl ester (4.7 ml, 37.5 mmol) in 15 ml of methanol is added drop wise. (Web site)
3. The crude product was crystallised from methanol to give 0.95g (5.0 mmol, 95%), mp 48-48.5�C.

Water

1. Finally, 0.29 ml (1.93 mmol) of TEMED, 0.426 g (2.6 mmol) of AIBN, and 100 ml of water were added to the reaction mixture. (Web site)
2. The oxime (20 mmol) was mixed with water (15 ml) containing sodium dithionite (28 mmol). (Web site)

Liter

1. A total of 42 percent of patients had a qualifying plasma total cholesterol level of less than 213 mg per deciliter (5.5 mmol per liter).
2. The mean total cholesterol level was 851 mg per deciliter (22.0 mmol per liter) at baseline.

Acetonitrile

1. N-(3-dimethylaminopropyl)acrylamide (50 mmol), ethyl 4-bromobutyrate (60 mmol), and acetonitrile (25 mL) were added into a 100-mL round-bottom flask. (Web site)

Toluene

1. To 46.0g (500 mmol) toluene is added 20.0g (150 mmol) AlCl3 under cooling in an ice bath.
2. Into a 500 ml evacuated flask containing 200 ml of toluene, 4 ml of propylene (50 mmol) was introduced at a temperature of 78.degree. (Web site)

Heated

1. Chlorodiisopropylsilane (2.155 g, 14.3 mmol, 1.1 equiv) was then added and the mixture was heated to reflux. (Web site)
2. A mixture of 1.00 g of acenaphthoquinone (5.5 mmol) and 4-allyl-2,6-diisopropylaniline (2.49 g, 11.1 mmol) in acetic acid (10 mL) was heated to reflux. (Web site)
3. Methanesulfonyl chloride (2.29 g, 20 mmol) is added and the reaction mixture is heated to reflux and maintained for 1 hour. (Web site)

Minutes

1. Next, 67.8 mmol of carbon dioxide was added thereto, so as to conduct a reaction for 30 minutes. (Web site)

Min

1. Potassium carbonate (2 g, 14.5 mmol) and butyliodide (1 ml, 8.8 mmol) were added and the reaction mixture was stirred for additionally 10 min. (Web site)
2. C.) CH.sub.2Cl.sub.2 (5.0 mL) solution Cap-55 (369 mg, 2.13 mmol) for about 50 min until the reaction mixture attained a tint of blue color. (Web site)

Solution

1. To the residue was added piperidine (5.73 mL, 58.1 mmol) and the solution was stirred at room temperature for 24 hours. (Web site)
2. To a stirred solution of 1 (2.82 g, 10 mmol) in CHCl.sub.3 (15 ml) is added N-chlorosuccinimide (1.5 g, 11 mmol) at room temperature under N.sub.2. (Web site)
3. To a solution of the resultant compound of Example 8 (400 mg, 1.09 mmol) in liquid ammonia (80 mL) was added sodium (150 mg, 6.5 mmol). (Web site)

Flask

1. To a flask fitted with a nitrogen inlet and a thermowell was added toluene (100 mL) and 2-amino-3-iodopyridine (8a, 10 g, 45.5 mmol). (Web site)
2. Two hundred fifty ml of liquid ammonia was condensed into the flask and 1.23 g (31.4 mmol) of sodium amide was added.
3. Separately, 1 mmol of adamantane, 0.05 mmol of 6-trifluoromethyl-1-hydroxybenzotriazole, and 5 ml of acetic acid were placed and were mixed in a flask. (Web site)

Mixture

1. The reaction mixture was heated at 60° C. for 1 h before ZnCl 2 (3.9 mL of 1.0 M solution in ether, 3.9 mmol) was added. (Web site)
2. The aqueous solution is stirred with a mixture of 69.8 ml of toluene and 65.7 mmol of triisooctylamine for 24 hours. (Web site)
3. The silanol (1.0-1.2 mmol) was added neat and the mixture was stirred for 10 minutes at room temperature. (Web site)

Triethylamine

1. Dicyclohexylcarbodiimide (1.2 mmol), triethylamine (2.0 mmol) and 4-dimethylaminopyridine (0.05 mmol) were placed in the reaction flask. (Web site)

Room Temperature

1. After cooling the reaction mixture to room temperature, acetic acid (6.2 g, 102.5 mmol) was added and the solvent (40 g) was removed.
2. C. was added DBU (6.19 g, 40.7 mmol) and the solution was allowed to warm to room temperature while stirring for 30 minutes. (Web site)
3. Methyl formate (0.5 ml, 8.0 mmol) was added and the reaction mixture was stirred at room temperature for 18 hours. (Web site)

Thf

1. A solution of the above bromomethyl compound (1.82 g, 5.0 mmol) in THF (20 ml) is added with stirring and the reaction mixture stirred for 4 h.
2. A solution of the above mesylate (0.45 g, 1.3 mmol) and N-methyl-N-propyl amine (0.33 mL, 3.25 mmol) in THF (50 mL) is heated at 55.degree.
3. To a stirred solution of 3 (2.0 g, 5 mmol) in THF (50 ml) is added LiBH.sub.4 (1.0 g excess) at 0.degree. (Web site)

Dropwise

1. C., and a solution of 37.0 mmol of triethylamine and 16.6 mmol of (-)-S-1,1'-bi(2-naphthol) 22 in 30 ml of dichloromethane is added dropwise. (Web site)
2. To the resulting aqueous ammonia mixture was dropwise added a solution of 21.6 g (77.8 mmol.) of ferrous sulfate 7 hydrates in 70 mL of water. (Web site)
3. After ten minutes of mixing, 5.00 g (42.0 mmol) of phenyl isocyanate (99% Aldrich) was added dropwise. (Web site)

Mmol

1. A solution of 3.1 ml (50 mmol) methyl formate in 10 ml methanol was then added dropwise at room temperature to the stirred solution. (Web site)
2. Under a nitrogen atmosphere, a slurry of 1.65 gm (10 mmol) phenylalanine in 4.0 ml (100 mmol) formamide was heated at 90.degree. (Web site)
3. A solution of the substrate 1 (5.0 mmol) in CH2Cl2 (8.0 mL) was added dropwise and the stirring continued at room temperature for the required time.

Categories

1. Dropwise
2. Thf
3. Room Temperature
4. Nature > Chemistry > Bases > Triethylamine
5. Nature > Matter > Materials > Mixture
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