Water → HCID 178441464、化合物

HRID 653717ノート

反応式

HRID 653717 の反応式
[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[C:8]2[C:25]([CH2:29][OH:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:31]=[N+:32]=[N-:33].[Na+].[Cl-].[NH4+].O>CN(C=O)C>[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]3[NH:33][N:32]=[N:31][N:24]=3)=[CH:15][CH:16]=2)[C:8]2[C:25]([CH2:29][OH:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 19792172HCID 19792172、化合物

生成物 1

HCID 178441464HCID 178441464、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]-7-hydroxymethylbenzimidazole (0.4 g), sodium azide (0.98 g) and ammonium chloride (0.8 g) in DMF (4 ml) was stirred for 4 days at 110°-120° C. To the reaction mixture was added water, which was extracted with ethyl acetate. The extract was washed with water and dried. After removal of the solvent, the residue was crystallized from ethyl acetate-methanol to give colorless needles, m.p. 152°-153° C.

後処理

  1. extractionwas extracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customAfter removal of the solvent
  5. customthe residue was crystallized from ethyl acetate-methanol
  6. customto give colorless needles, m.p. 152°-153° C.

出典と根拠

ORDレコード
ord-6024df42c90e4a2696b778fc5ffba0ea
出典データセット
uspto-grants-1992_07
特許番号
US05128356

反応ノート

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