Pyridine → [1-(3,4-Dimethoxyphenyl)-4-oxocyclohexyl]methyl acetate

HRID 1576220노트

반응식

HRID 1576220 반응식
[OH:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.N1C=CC=CC=1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>O>[C:26]([O:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:4][CH2:5][C:6](=[O:9])[CH2:7][CH2:8]1)(=[O:28])[CH3:27]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 215146714-(3,4-Dimethoxyphenyl)-4-(hydroxymethyl)cyclohexan-1-one

생성물 1

HCID 21514706[1-(3,4-Dimethoxyphenyl)-4-oxocyclohexyl]methyl acetate수율 57%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The 4-hydroxymethyl-4-(3,4-dimethoxyphenyl)cyclohexanone is dissolved in 20 ml. of pyridine and 10 ml. of acetic anhydride. After about 20 hours of standing at room temperature, the mixture is poured into ice and water. The gum that precipitates is extracted with ether. The organic layer is washed successively with water, 2.5 N hydrochloric acid, water and brine, and evaporated to dryness to give 6.43 g. (57% yield) of 4-acetoxymethyl-4-(3,4-dimethoxyphenyl)cyclohexanone, as an amorphous gum.

후처리

  1. customThe gum that precipitates
  2. extractionis extracted with ether
  3. washThe organic layer is washed successively with water, 2.5 N hydrochloric acid, water and brine
  4. customevaporated to dryness
  5. customto give 6.43 g

출처 및 근거

ORD 기록
ord-4393d21c72bb42839169441d1910a593
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03979444

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