Imidazole → HCID 131730158、化合物

HRID 1806971ノート

反応式

HRID 1806971 の反応式
[CH2:1]([C:3](CO)([CH2:7][CH3:8])[CH2:4][C:5]#N)[CH3:2].N1[CH:15]=[CH:14][N:13]=C1.[C:16]([Si:20](C)(C)Cl)([CH3:19])([CH3:18])[CH3:17].[OH2:24].Cl[CH2:26]Cl>>[C:16]([SiH2:20][O:24][C:1]([CH3:2])([CH3:26])[C:3]([CH2:4][CH3:5])([CH2:7][CH3:8])[CH2:15][C:14]#[N:13])([CH3:19])([CH3:18])[CH3:17]

参加物

6

反応物 5

HCID 795ImidazoleHCID 962WaterHCID 6344DichloromethaneHCID 28928tert-Butyldimethylsilyl chlorideHCID 866404003-Ethyl-3-(hydroxymethyl)pentanenitrile

生成物 1

HCID 131730158HCID 131730158、化合物収率 74%

実験手順

Step C To the solution of 3-ethyl-3-hydroxymethyl-pentanenitrile (1.7 g, 12 mmol) and imidazole (1.2 g, 18 mmol) in dichloromethane (80 mL) was added tert-butyldimethylchlorosilane (2 g, 13 mmol). The reaction mixture was stirred at room temperature for 2 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-silanyloxymethyl)-3-ethyl-pentanenitrile as a colorless oil (2.28 g, 74%).

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-687b4f5937e140e285f18dfbeb95fcc9
出典データセット
uspto-grants-2013_01
特許番号
US08354444B2

反応ノート

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