Hydrazine → 4-Chloro-6-hydrazinyl-2-(methylsulfanyl)pyrimidine

HRID 2065503

反応式

HRID 2065503 の反応式
[NH2:1][NH2:2].[Cl:3][C:4]1[CH:9]=[C:8](Cl)[N:7]=[C:6]([S:11][CH3:12])[N:5]=1>ClCCl>[Cl:3][C:4]1[N:5]=[C:6]([S:11][CH3:12])[N:7]=[C:8]([NH:1][NH2:2])[CH:9]=1

参加物

4

反応物 2

HCID 9321HydrazineHCID 805314,6-Dichloro-2-(methylthio)pyrimidine

生成物 1

HCID 14845464-Chloro-6-hydrazinyl-2-(methylsulfanyl)pyrimidine収率 64.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

Referring to Scheme 2, anhydrous hydrazine (164 mg, 162 μl, 5.1 mmol) and dichloromethane (3 ml) were cooled to −78° C. 4,6-Dichloro-2-(methylthio)pyrimidine (1 g, 5.1 mmol) was slowly added. The mixture was allowed to stir for 10 minutes then the bath was replaced with an ice bath and the solution allowed to slowly reach 0° C. The precipitate was filtered and washed with DCM. 1-(6-Chloro-2-(methylthio)pyrimidin-4-yl)hydrazine (624 mg, 64%) was obtained. [M+H] calc'd for C5H7ClN4S, 191; found, 191.

後処理

  1. customthe bath was replaced with an ice bath
  2. customallowed to slowly reach 0° C
  3. filtrationThe precipitate was filtered
  4. washwashed with DCM

出典と根拠

ORDレコード
ord-3e14dd27720a428dad453f76d6f57fa7
出典データセット
uspto-grants-2012_10
特許番号
US08288536B2

関連ノート

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