Chloropyrazine → HCID 57227784、化合物

HRID 2260805

反応式

HRID 2260805 の反応式
[CH3:1][N:2]1[CH2:7][C@@H:6]2[CH2:8][C@H:3]1[CH2:4][NH:5]2.Cl[C:10]1[CH:15]=[N:14][CH:13]=[CH:12][N:11]=1>C(Cl)Cl>[CH3:1][N:2]1[CH2:7][C@@H:6]2[CH2:8][C@H:3]1[CH2:4][N:5]2[C:10]1[CH:15]=[N:14][CH:13]=[CH:12][N:11]=1

参加物

4

反応物 2

HCID 73277ChloropyrazineHCID 11029795(1S,4S)-2-Methyl-2,5-diazabicyclo[2.2.1]heptane

生成物 1

HCID 57227784HCID 57227784、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

A solution of 2.1 g of (S,S)-2-methyl-2,5-diazabicyclo[2.2.1]heptane prepared by the procedure of U. Jordis et al, Synthesis, 1990, 925, and 1.8 ml of 2-chloropyrazine in 8 ml of diazabicyclo[3.6.0]undecene-5 is heated to approximately 80° C. for 2 hours. The reaction solution is cooled, diluted with 100 ml of methylene chloride and washed with 30 ml of 5N aqueous sodium hydroxide. The organic layer is dried and concentrated in vacuo to dryness. The residue is purified by chromatography (aluminum oxide, Activity Grade 2.5; methylene chloride to 5% methyl alcohol/methylene chloride) to give 2.1 g of the desired product as a pale yellow oil:

後処理

  1. temperatureThe reaction solution is cooled
  2. washwashed with 30 ml of 5N aqueous sodium hydroxide
  3. customThe organic layer is dried
  4. concentrationconcentrated in vacuo to dryness
  5. customThe residue is purified by chromatography (aluminum oxide, Activity Grade 2.5; methylene chloride to 5% methyl alcohol/methylene chloride)

出典と根拠

ORDレコード
ord-19199d6472b0477a9985a98b6cfa98b2
出典データセット
uspto-grants-1995_12
特許番号
US05478939

関連ノート

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