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Cyanogen Bromide → HCID 58045867、化合物

HRID 1524448
ノート
印刷プレビュー

反応式

HRID 1524448 の反応式
[N:1]1([C:6]2[N:11]=[N:10][C:9]([NH:12][NH2:13])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.C([O-])(=O)C.[Na+].[N:19]#[C:20]Br.[OH-].[Na+]>C(O)(=O)C.O>[N:1]1([C:6]2[CH:7]=[CH:8][C:9]3[N:10]([C:20]([NH2:19])=[N:13][N:12]=3)[N:11]=2)[CH:5]=[CH:4][N:3]=[CH:2]1
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 10476Cyanogen BromideHCID 14798Sodium HydroxideHCID 517045Sodium AcetateHCID 30313233-hydrazinyl-6-(1H-imidazol-1-yl)pyridazine

生成物 1

HCID 58045867HCID 58045867、化合物収率 11.6%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 962
Water
溶媒

反応条件

温度
0 °C

実験手順

(6-Imidazol-1-ylpyridazin-3-yl)hydrazine (500 mg) were initially charged in a mixture of acetic acid (4 ml) and water (8 ml) with addition of sodium acetate (232 mg) at RT while stirring. Thereafter, the mixture was cooled to 0° C. and cyanogen bromide (330 mg) was introduced in portions. After stirring for 2.5 h, the mixture was left to stand overnight. After cooling to 0° C., the mixture was alkalized with 10 M sodium hydroxide solution and extracted repeatedly with EA. The combined EA phases were dried over sodium sulfate, filtered and concentrated. 66 mg of the title compound were isolated.

後処理

  1. stirringAfter stirring for 2.5 h
  2. waitthe mixture was left
  3. temperatureAfter cooling to 0° C.
  4. extractionextracted repeatedly with EA
  5. dry with materialThe combined EA phases were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-697ead6700bb4c6a8c9536616655cf7c
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09079906B2

反応ノート

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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