Methanol → HCID 57455338, 화합물

HRID 1093930노트

반응식

HRID 1093930 반응식
[C:1]([CH2:3][CH2:4][CH2:5][OH:6])#[N:2].C(N(CC)CC)C.[C:14](Cl)([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.CO>ClCCl>[C:14]([O:6][CH2:5][CH2:4][CH2:3][C:1]#[N:2])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 2207054-Hydroxybutanenitrile

생성물 1

HCID 57455338HCID 57455338, 화합물수율 61.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-cyano-1-n-propanol (16.85 g, 198 mmol, prepared by method of Blicke, et al., J. Org. Chem. 1961, 26, 3685) in dichloromethane (250 mL) were added triethylamine (80.1 g, 792 mmol) and trityl chloride (82.8 g, 297 mmol) at room temperature and the mixture was stirred for 16 h. To the reaction mixture was added methanol (25 mL) and stirred for 1 h. After concentration, the residue was purified on a column of silica gel using ethyl acetate and hexanes as eluent to give 40 g (61.7%) of the desired product.

후처리

  1. stirringstirred for 1 h
  2. concentrationAfter concentration
  3. customthe residue was purified on a column of silica gel

출처 및 근거

ORD 기록
ord-ad6966b204d14c8f889ce5273d06e1c0
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08133870B2

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