Hydrochloric Acid → HCID 67689502、化合物

HRID 258438ノート

反応式

HRID 258438 の反応式
[C:1]([O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)(=[O:5])[C@H:2]([CH3:4])[OH:3].C(N(CC)CC)C.C(Cl)Cl.[C:23](Cl)(=[O:26])[CH:24]=[CH2:25].Cl>>[C:23]([O:3][C@@H:2]([CH3:4])[C:1]([O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:5])(=[O:26])[CH:24]=[CH2:25]

参加物

6

反応条件

温度
-20 °C

実験手順

To a mixture of 10.1 g (58.5 mmol) of cyclohexyl (s)-(-)-lactate, 8.1 g (80.4 mmol) of triethylamine and ml of methylene chloride, 5.7 ml (70.2 mmol) of acryloyl chloride was added dropwise at a temperature of -20° C., and the mixture was stirred at -20° C. for 5.5 hours. On ice cooling, 1N hydrochloric acid was added to the reaction mixture to separate an organic layer, and an aqueous layer was extracted with methylene chloride. Organic layers were combined and washed with successive, saturated sodium bicarbonate solution, water, and saturated sodium chloride solution. The solution was dried over anhydrous magnesium sulfate and filtered, the solvent was distilled off, and 13.5 g of crude (S)-cyclohexyl 2-propenoyloxypropionate was obtained.

後処理

  1. additionwas added dropwise at a temperature of -20° C.
  2. customto separate an organic layer
  3. extractionan aqueous layer was extracted with methylene chloride
  4. washwashed with successive, saturated sodium bicarbonate solution, water, and saturated sodium chloride solution
  5. dry with materialThe solution was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-78e5e1a0462341f9aa32412978b311ed
出典データセット
uspto-grants-1993_11
特許番号
US05266728

反応ノート

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