Imidazole → 2-(Tert-butyldiphenylsilyloxymethyl)imidazole

HRID 1251875

反応式

HRID 1251875 の反応式
[OH:1][CH2:2][C:3]1[NH:4][CH:5]=[CH:6][N:7]=1.N1C=CN=C1.[Si:13](Cl)([C:26]([CH3:29])([CH3:28])[CH3:27])([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CN(C=O)C>[Si:13]([O:1][CH2:2][C:3]1[NH:4][CH:5]=[CH:6][N:7]=1)([C:26]([CH3:29])([CH3:28])[CH3:27])([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 795ImidazoleHCID 94078tert-ButyldiphenylchlorosilaneHCID 5668301H-Imidazole-2-methanol

生成物 1

HCID 536766582-(Tert-butyldiphenylsilyloxymethyl)imidazole収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-hydroxymethylimidazole (1.96 g ; 0.02 mole), imidazole (3.4 g; 0.05 mole), tert-butyldiphenylsilyl chloride (6.6 g; 0.024 mole) in DMF (20 ml) was stirred under an argon atmosphere for 16 hours. The mixture was extracted with ethyl acetate and purified by flash column chromatography eluting with a gradient 50-70% ethyl acetate/petroleum ether to give 2-(tert-butyldiphenylsilyloxymethyl)imidazole as a solid.

後処理

  1. extractionThe mixture was extracted with ethyl acetate
  2. custompurified by flash column chromatography
  3. washeluting with a gradient 50-70% ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-629180fcd2854c04ab9ada2162252392
出典データセット
uspto-grants-2002_01
特許番号
US06342765B1

関連ノート

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