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Water → HCID 178441449、化合物

HRID 1655448
ノート
印刷プレビュー

反応式

HRID 1655448 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[CH:25]=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:29]=[N+:30]=[N-:31].[Na+].[Cl-].[NH4+].O>CN(C=O)C.C(OCC)(=O)C>[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:31][N:30]=[N:29][N:24]=3)=[CH:13][CH:12]=2)[C:8]2[CH:25]=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]
参加物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 962WaterHCID 25517Ammonium Chloride2 回HCID 33557Sodium Azide2 回HCID 197921082-Butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole

生成物 1

HCID 178441449HCID 178441449、化合物収率 41%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole (1.8 g), sodium azide (0.98 g) and ammonium chloride (0.80 g) was stirred in DMF (6 ml) at 110° C. for 5 days, while supplementing sodium azide (1.6 g), ammonium chloride (1.3 g) and DMF (5 ml) to the reaction system. To the reaction mixture were added water and ethyl acetate, and precipitating crystals were collected by filtration. The organic layer of the filtrate was washed with water, dried and concentrated under reduced pressure to give crude crystals. These crystals were combined with the crystals obtained previously, this was followed by recrystallization from ethyl acetate - methanol to afford colorless prisms (0.82 g, 41%), m.p. 235-236° C.

後処理

  1. customprecipitating crystals
  2. filtrationwere collected by filtration
  3. washThe organic layer of the filtrate was washed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customto give crude crystals
  7. customobtained previously
  8. customthis was followed by recrystallization from ethyl acetate - methanol

出典と根拠

ORDレコード
ord-3ae554d6481c4bb7bff7dc0396bb5543
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…

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