Sulfuryl chloride → Ethyl 2-chloro-3-oxo-4-phenylbutyrate

HRID 1173779

반응식

HRID 1173779 반응식
[O:1]=[C:2]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].S(Cl)([Cl:19])(=O)=O>C(Cl)Cl>[Cl:19][CH:3]([C:2](=[O:1])[CH2:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 225855Ethyl 3-oxo-4-phenylbutanoate

생성물 1

HCID 11601176Ethyl 2-chloro-3-oxo-4-phenylbutyrate수율 86.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
20 °C

실험 절차

Ethyl 3-oxo-4-phenylbutyrate (4.8 g, 23 mmol) and methylene chloride (48 ml) were mixed, and sulfuryl chloride (3.1 g, 1 equivalent) was gradually added thereto dropwise. After the addition, the mixture was stirred at 20° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and saturated aqueous solution of sodium hydrogencarbonate (10 ml) was added, and extraction was carried out with ethyl acetate (20 ml). The solvent was evaporated away under reduced pressure and drying was carried out in vacuum to obtain the title compound as a yellow oil (4.8 g, yield: 86%).

후처리

  1. additionAfter the addition
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated aqueous solution of sodium hydrogencarbonate (10 ml)
  3. additionwas added
  4. extractionextraction
  5. customThe solvent was evaporated away under reduced pressure
  6. customdrying

출처 및 근거

ORD 기록
ord-e6baa6b5b8594ff7abbfbb4adeb29779
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834190B2

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