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Water → HCID 59295129、化合物

HRID 2233034
ノート
印刷プレビュー

反応式

HRID 2233034 の反応式
[Cl:1][C:2]1[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])=[N:4][CH:5]=[CH:6][N:7]=1.N1C=CC=CC=1.[Br:22]Br.O>CC(O)=O>[Br:22][C:6]1[N:7]=[C:2]([Cl:1])[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:12])([F:13])[F:14])=[N:4][CH:5]=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

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 24408BromineHCID 58446973HCID 58446973、化合物

生成物 1

HCID 59295129HCID 59295129、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 2.40 g of the product of Step A and 1.97 g of pyridine in AcOH (10.0 mL) at 0° C. was stirred as a solution of 1.92 g of bromine in AcOH (1.0 mL) was added dropwise. The resulting mixture was stirred at 0° C. for one h and then warmed to ambient temperature and stirred for an additional 16 h. The reaction mixture was poured into water and extracted with EtOAc (2×). The combined organic extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to an oil that was purified by silica gel chromatography to provide trifluoroacetic acid N′-(5-bromo-3-chloro-pyrazin-2-yl)-hydrazide as a white solid. MS (M+H+)=320.1.

後処理

  1. additionwas added dropwise
  2. temperaturewarmed to ambient temperature
  3. stirringstirred for an additional 16 h
  4. extractionextracted with EtOAc (2×)
  5. washThe combined organic extracts were washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to an oil that
  9. customwas purified by silica gel chromatography

出典と根拠

ORDレコード
ord-7c40a0dece594b1b8479acefcc7612d6
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709473B2

反応ノート

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