Water → HCID 21474599, 화합물

HRID 1756435노트

반응식

HRID 1756435 반응식
[H-].[Na+].[C:3]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=[O:11])=[CH:8][CH:7]=1)(=[O:5])[CH3:4].[CH2:15](Br)[CH:16]=[CH2:17].O>CN(C=O)C>[C:3]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([O:12][CH2:17][CH:16]=[CH2:15])=[O:11])=[CH:8][CH:7]=1)(=[O:5])[CH3:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 7841Allyl bromideHCID 114704-Acetylbenzoic AcidHCID 24758Sodium hydride

생성물 1

HCID 21474599HCID 21474599, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

1.65 g (55 mmol) of sodium hydride (80% in oil ) and 50 ml of DMF are introduced under a stream of nitrogen into a round-bottomed flask. 8.2 g (50 mmol) of 4-acetylbenzoic acid, dissolved in 100 ml of DMF, are added dropwise and the mixture is stirred at room temperature until gaseous evolution has ceased. 4.6 ml (55 mmol) of allyl bromide are then introduced and the mixture is stirred at room temperature for 24 hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column, eluting with a mixture of dichloromethane and hexane (80:20). After evaporation of the solvents, 7.2 g (71 % ) of allyl ester are collected in the form of a colorless oil.

후처리

  1. additionare added dropwise
  2. stirringthe mixture is stirred at room temperature for 24 hours
  3. extractionthe mixture is extracted with ethyl ether
  4. customthe organic phase is separated after settling
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue obtained
  8. customis purified by chromatography on a silica column
  9. washeluting with a mixture of dichloromethane and hexane (80:20)
  10. customAfter evaporation of the solvents, 7.2 g (71 % ) of allyl ester
  11. customare collected in the form of a colorless oil

출처 및 근거

ORD 기록
ord-65f243a23ecb4f42ba133e0ed3b3d88a
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05439925

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