Chlorotrimethylsilane → 1-Dimethylcarbamoyl-4-(3-trimethylsilyloxypropyl)imidazole

HRID 1032333

反応式

HRID 1032333 の反応式
[CH3:1][N:2]([CH3:14])[C:3]([N:5]1[CH:9]=[C:8]([CH2:10][CH2:11][CH2:12][OH:13])[N:7]=[CH:6]1)=[O:4].C(N(CC)CC)C.Cl[Si:23]([CH3:26])([CH3:25])[CH3:24]>C(#N)C.CCOCC>[CH3:14][N:2]([CH3:1])[C:3]([N:5]1[CH:9]=[C:8]([CH2:10][CH2:11][CH2:12][O:13][Si:23]([CH3:26])([CH3:25])[CH3:24])[N:7]=[CH:6]1)=[O:4]

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 145750511-Dimethylcarbamoyl-4-(3-hydroxypropyl)-imidazole

生成物 1

HCID 112772221-Dimethylcarbamoyl-4-(3-trimethylsilyloxypropyl)imidazole

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

1-Dimethylcarbamoyl-4-(3-hydroxypropyl)-imidazole (19.8 g, 0.10 mole) and triethylamine (15 g, 0.15 mole) are dissolved in acetonitrile (100 mL) and the solution is stirred and cooled in an ice bath during the dropwise addition of chlorotrimethylsilane (11.9 g, 0.11 mole). The reaction is stirred at ice-bath temperature for 1 hour and is subsequently allowed to stand at ambient temperature for 15 hours. The mixture is diluted with ether (500 mL), filtered, and the solvent is evaporated to give 1-dimethylcarbamoyl-4-(3-trimethylsilyloxypropyl)imidazole as an oil; NMR (imidazole protons): 2.2 (s) and 3.05 (s) ppm.

後処理

  1. stirringThe reaction is stirred at ice-bath temperature for 1 hour
  2. filtrationfiltered
  3. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-7cfb334db5824ce4b6073ad9f6ea7411
出典データセット
uspto-grants-1990_09
特許番号
US04957931

関連ノート

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