Water → HCID 19905431, 화합물

HRID 2371916노트

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HRID 2371916 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[C:11]([C:13]1[N:14]([S:20](=[O:25])(=[O:24])[N:21]([CH3:23])[CH3:22])[CH:15]=[C:16]([CH2:18][OH:19])[N:17]=1)#[N:12].C(N(CC)CC)C.O>ClCCl>[C:11]([C:13]1[N:14]([S:20](=[O:24])(=[O:25])[N:21]([CH3:22])[CH3:23])[CH:15]=[C:16]([CH2:18][O:19][C:6](=[O:7])[C:5]2[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][CH:4]=2)[N:17]=1)#[N:12]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 199054352-Cyano-4-(hydroxymethyl)-N,N-dimethyl-1H-imidazole-1-sulfonamide

생성물 1

HCID 19905431HCID 19905431, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Chlorobenzoyl chloride (0.83 g) was added to a solution of 2-cyano-4-hydroxymethyl-1-(dimethylsulphamoyl)-imidazole (1.5 g) in dichloromethane (50 ml), containing triethylamine (1.0 ml) at 0°. The mixture was stirred for 45 minutes whilst the temperature was allowed to rise to room temperature. The mixture was added to water and the organic phase was separated, washed, dried and concentrated under reduced pressure. The residue was recrystallised from a mixture of diisopropyl ether and ethyl acetate to give 2-cyano-4-(4-chlorobenzoyloxy-methyl)-1-(dimethylsulphamoyl)imidazole, m.p. 94≥-96°. (Compound 1)

후처리

  1. customto rise to room temperature
  2. customthe organic phase was separated
  3. washwashed
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallised from a mixture of diisopropyl ether and ethyl acetate

출처 및 근거

ORD 기록
ord-609986e4b6354dc9a9729ca95b02c0cf
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05096915

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