Water → HCID 19905431、化合物

HRID 2371916ノート

反応式

HRID 2371916 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 19905431HCID 19905431、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-609986e4b6354dc9a9729ca95b02c0cf
出典データセット
uspto-grants-1992_03
特許番号
US05096915

反応ノート

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