Ethyl chloroformate → Ethyl (1-methyl-1H-imidazol-2-yl)carbamate

HRID 741713노트

반응식

HRID 741713 반응식
[C:1](Cl)(=[O:5])[O:2][CH2:3][CH3:4].Cl.[NH2:8][C:9]1[N:10]([CH3:14])[CH:11]=[CH:12][N:13]=1>N1C=CC=CC=1>[CH2:3]([O:2][C:1]([NH:8][C:9]1[N:10]([CH3:14])[CH:11]=[CH:12][N:13]=1)=[O:5])[CH3:4]

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 101540761-Methyl-1H-imidazol-2-amine hydrochloride

생성물 1

HCID 15837347Ethyl (1-methyl-1H-imidazol-2-yl)carbamate

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
100 °C

실험 절차

Ethyl chlorocarbonate (0.6 g) was added to a solution of 2-amino-1-methylimidazole hydrochloride (0.3 g) in pyridine (5 ml), and the mixture was stirred under heating at 100° C. for 2 hours. The solvent was evaporated under reduced pressure, the residue was dissolved in water, and sodium carbonate was added until the solution became alkaline. The solvent was evaporated under reduced pressure, and then the residue was purified by column chromatography on silica gel (eluent: chloroform) to give 2-ethoxycarbonylamino-1-methylimidazole. This compound was dissolved in dichloromethane, and 4N hydrochloric acid-ethyl acetate (2 ml) was added to form its hydrochloric acid salt. The resulting crude crystals were washed with ether to give 2-ethoxycarbonylamino-1-methylimidazole hydrochloride (0.29 g, Yield: 56%) as colorless prisms.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in water
  3. additionsodium carbonate was added until the solution
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: chloroform)

출처 및 근거

ORD 기록
ord-9d6234d79398474d947f533661f03d54
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05552427

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