Diethyl Ether → Benzyl (1-methyl-1H-imidazol-2-yl)carbamate

HRID 741714ノート

反応式

HRID 741714 の反応式
Cl.[NH2:2][C:3]1[N:4]([CH3:8])[CH:5]=[CH:6][N:7]=1.[CH2:9]([O:16][C:17](Cl)=[O:18])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCOCC>[OH-].[Na+]>[CH2:9]([O:16][C:17]([NH:2][C:3]1[N:4]([CH3:8])[CH:5]=[CH:6][N:7]=1)=[O:18])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 10387Benzyl chloroformateHCID 101540761-Methyl-1H-imidazol-2-amine hydrochloride

生成物 1

HCID 19426850Benzyl (1-methyl-1H-imidazol-2-yl)carbamate

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

2-Amino-1-methylimidazole hydrochloride (0.3 g) was dissolved in 1N sodium hydroxide solution (5 ml ). Benzyloxycarbonyl chloride (0.43 g) and ether (2 ml ) were added, and the mixture was stirred for 1 hour. The product was extracted with ethyl acetate, the extract was washed with water and aqueous saturated sodium chloride solution and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. Diethyl ether-hexane was added to the resulting residue for crystallization, and the crystals were separated by filtration. The crystals of 2-benzyloxycarbonylamino-1-methylimidazole thus obtained was dissolved in chloroform, and 4N hydrochloric acid-ethyl acetate (0.5 ml) was added to form its hydrochloric acid salt. The crude crystals thus obtained were washed with ether to give 2-benzyloxycarbonylamino-1-methylimidazole hydrochloride (0.2 g, Yield: 30% ) as white powder.

後処理

  1. extractionThe product was extracted with ethyl acetate
  2. washthe extract was washed with water and aqueous saturated sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. additionDiethyl ether-hexane was added to the resulting residue for crystallization
  6. customthe crystals were separated by filtration

出典と根拠

ORDレコード
ord-634ad6d74d3247fdba90e9c2cebf4ff9
出典データセット
uspto-grants-1996_09
特許番号
US05552427

反応ノート

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