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

HRID 1032333

반응식

HRID 1032333 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-7cfb334db5824ce4b6073ad9f6ea7411
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04957931

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