Methanol → HCID 57455338、化合物

HRID 1093930ノート

反応式

HRID 1093930 の反応式
[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

参加物

6

反応物 4

HCID 887MethanolHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 2207054-Hydroxybutanenitrile

生成物 1

HCID 57455338HCID 57455338、化合物収率 61.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-ad6966b204d14c8f889ce5273d06e1c0
出典データセット
uspto-grants-2012_03
特許番号
US08133870B2

反応ノート

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