Water → 1,2-Butanediol diacetate

HRID 274828

반응식

HRID 274828 반응식
[CH2:1]([OH:6])[CH:2]([OH:5])[CH2:3][CH3:4].N1[CH:12]=[CH:11]C=CC=1.[C:13](Cl)(=[O:15])[CH3:14].[OH2:17]>C1(C)C=CC=CC=1>[C:13]([O:6][CH2:1][CH:2]([O:5][C:11](=[O:17])[CH3:12])[CH2:3][CH3:4])(=[O:15])[CH3:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 6367Acetyl chlorideHCID 114291,2-Butanediol

생성물 1

HCID 99204991,2-Butanediol diacetate

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a mixture of 0.34 g of optically active 1,2-butanediol, 5 ml of toluene and 2.5 ml of pyridine, 1.2 g of acetyl chloride was added dropwise in an ice bath and stirred for two hours. 10 ml of water and 10 ml of toluene were added to the reaction mixture and stirred. The obtained solution was washed with 2N sodium hydroxide and then with water. The toluene solution dried over anhydrous magnesium sulfate. Toluene was distilled away from the solution under reduced pressure, the residue was purified with a chromatograph over silica gel, and 1,2-butanediol diacetate was obtained. The obtained compound had a gas chromatographic purity of 95.0%. It showed a specific rotation of [α]D30 +14.8(c=1.12, CHCl3).

후처리

  1. additionwas added dropwise in an ice bath
  2. stirringstirred
  3. washThe obtained solution was washed with 2N sodium hydroxide
  4. dry with materialThe toluene solution dried over anhydrous magnesium sulfate
  5. distillationToluene was distilled away from the solution under reduced pressure
  6. customthe residue was purified with a chromatograph over silica gel

출처 및 근거

ORD 기록
ord-fabb0a4b81084ed185708f110ddee3ad
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391494

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