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Hydrochloric Acid → HCID 178441455、化合物

HRID 1655479
ノート
印刷プレビュー

反応式

HRID 1655479 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]([CH3:29])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:30]=[N+:31]=[N-:32].[Na+].[Cl-].[NH4+].Cl>CN(C=O)C.O>[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]3[NH:32][N:31]=[N:30][N:24]=3)=[CH:13][CH:12]=2)[C:8]2[C:25]([CH3:29])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 19792145HCID 19792145、化合物

生成物 1

HCID 178441455HCID 178441455、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
115 °C

実験手順

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]-7-methylbenzimidazole (0,5 g), sodium azide (1.3 g) and ammonium chloride (1.1 g) in DMF (5 ml) was stirred for 3.5 days at 110-120° C. To the reaction mixture was added water, which was made acidic (pH 3-4) with 1N-HCl, followed by extraction with ethyl acetate. The organic layer was washed with water and dried. The solvent was distilled off, and the residue was purified by column chromatography on silica gel to give crystals. Recrystallization from ethyl acetate-methanol afforded colorless crystals (0.36 g, 62%),

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by column chromatography on silica gel
  6. customto give crystals
  7. customRecrystallization from ethyl acetate-methanol afforded colorless crystals (0.36 g, 62%)

出典と根拠

ORDレコード
ord-49811bd16a82404d9e36a0d9b0b39a45
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250554

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート