Water → HCID 178418381, 화합물

HRID 1737934

반응식

HRID 1737934 반응식
[C:1]([O:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]2[CH:16]=[CH:15][C:14]([CH2:17]Cl)=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:25]([NH:27][CH2:28][CH3:29])[CH3:26].O>CN(C)C=O>[C:1]([O:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]2[CH:16]=[CH:15][C:14]([CH2:17][N:27]([CH2:28][CH3:29])[CH2:25][CH3:26])=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 8021DiethylamineHCID 11430Potassium CarbonateHCID 178418412HCID 178418412, 화합물

생성물 1

HCID 178418381HCID 178418381, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A solution of 1 g (3.75 mmol) of trans-O-acetyl-4-(4-chloromethylphenyl)-cyclohexanol in 10 ml of dimethylformamide is mixed with 0.52 g (3.75 mmol) of potassium carbonate and 0.27 g (3.75 mmol) of diethylamine. This mixture is heated to 50° C. for 6 hours with stirring, then water is added and the mixture is extracted with methylene chloride. The organic phase is dried, evaporated down in vacuo and the residue remaining is purified by column chromatography (aluminium oxide basic, activity stage III, ICN; petroleum ether/ethyl acetate=15:1). Colourless oil. Yield: 0.79 g (69% of theory)

후처리

  1. extractionthe mixture is extracted with methylene chloride
  2. customThe organic phase is dried
  3. customevaporated down in vacuo
  4. customthe residue remaining is purified by column chromatography (aluminium oxide basic, activity stage III, ICN; petroleum ether/ethyl acetate=15:1)

출처 및 근거

ORD 기록
ord-f5d03a55081842869fcad0b1d06ce12d
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962507

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