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

HRID 2065503

반응식

HRID 2065503 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3e14dd27720a428dad453f76d6f57fa7
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288536B2

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