Imidazole → 3-{[Tert-butyl(dimethyl)silyl]oxy}-2,2-dimethylpropan-1-ol

HRID 417252ノート

反応式

HRID 417252 の反応式
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].N1C=CN=C1.[C:13]([Si:17]([CH3:20])([CH3:19])Cl)([CH3:16])([CH3:15])[CH3:14].O>ClCCl>[C:13]([Si:17]([CH3:20])([CH3:19])[O:4][CH2:3][C:2]([CH3:7])([CH3:1])[CH2:5][OH:6])([CH3:16])([CH3:15])[CH3:14]

参加物

6

反応物 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 31344Neopentyl glycol

生成物 1

HCID 590121383-{[Tert-butyl(dimethyl)silyl]oxy}-2,2-dimethylpropan-1-ol収率 881.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2,2-dimethyl-propane-1,3-diol (Aldrich) (10 g, 96 mmol) and imidazole (9.8 g, 140 mmol) in dichloromethane (200 mL) was added tert-butyldimethylchlorosilane (15.9 g, 10.6 mmol). The reaction mixture was stirred at room temperature for 0.5 h. Water was added. The organic layer was separated, the aqueous layer was then extracted with dichloromethane. The combined organic layers were washed with brine, dried over MgSO4, concentrated to give 3-(tert-butyl-dimethyl-silanyloxy)-2,2-dimethyl-propan-1-ol as a colorless oil (20.4 g, 97%).

後処理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was then extracted with dichloromethane
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6c12aae24f134e73af2acd0c2417f0cb
出典データセット
uspto-grants-2012_01
特許番号
US08088815B2

反応ノート

読み込み中…