Hydrazine hydrate (1:1) → 4-Chloro-6-hydrazinylpyrimidine

HRID 220092

反応式

HRID 220092 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.O.[NH2:10][NH2:11]>CC(O)C>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([NH:10][NH2:11])[CH:7]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 709434,6-Dichloropyrimidine

生成物 1

HCID 2472224-Chloro-6-hydrazinylpyrimidine収率 94%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 4,6-dichloro-pyrimidine (18.68 g, 125 mmol), hydrazine monohydrate (18.28 mL, 376 mmol), and 2-propanol (300 mL) was stirred at room temperature for 3 hours. The reaction mixture was concentrated, triturated with water, and filtered. The solid was washed with water, air-dried to give (6-chloro-pyrimidin-4-yl)-hydrazine (16.97 g, Yield 94%): 1H NMR 400 MHz (d6-DMSO) δ 8.83 (s, 1H), 8.17 (s, 1H), 6.76 (s, 1H), 4.50 (s, 2H); MS m/z 145.02 (M+1).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customtriturated with water
  3. filtrationfiltered
  4. washThe solid was washed with water
  5. customair-dried

出典と根拠

ORDレコード
ord-6203da0ef3b845a3a7b5292d779c13c8
出典データセット
uspto-grants-2012_06
特許番号
US08202876B2

関連ノート

読み込み中…