Dimethylformamide → HCID 67287398, 화합물

HRID 74986노트

반응식

HRID 74986 반응식
[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([O:15][CH3:16])[CH:10]1[OH:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18]([Si:22](Cl)([CH3:24])[CH3:23])([CH3:21])([CH3:20])[CH3:19].CN(C=O)C.N1C=NCC=1>CN(C)C1C=CN=CC=1.CCOCC>[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([O:15][CH3:16])[CH:10]1[O:17][Si:22]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:24])[CH3:23])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 127446564H-ImidazoleHCID 151872871-Benzyloxy-3-methoxy-cyclohexan-2-ol2회

생성물 1

HCID 67287398HCID 67287398, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 1-benzyloxy-3-methoxy-cyclohexan-2-ol, 51d, (2.31 g, 9.78 mmol), tert-butyl-chlorodimethyl-silane (2.21 g, 2.73 mL, 14.66 mmol) in 20 dry DMF at room temperature was added 4H-imidazole (1.997 g, 29.33 mmol) and a catalytic amount of 4-dimethylaminopyridine (0.12 g, 0.98 mmol). The resulting mixture was stirred at room temperature overnight. It was then diluted with ether, washed with water, aqueous saturated citric acid solution and water again. The organic phase was dried with MgSO4, filtered and concentrated in vacuo. The colorless crude oil was used directly in the next step without further purification.

후처리

  1. washwashed with water, aqueous saturated citric acid solution and water again
  2. dry with materialThe organic phase was dried with MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe colorless crude oil was used directly in the next step without further purification

출처 및 근거

ORD 기록
ord-3ffd812bbcf141c3bf50331d958cc488
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829007B2

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