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

HRID 2389764

반응식

HRID 2389764 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[NH2:11][NH2:12]>C1COCC1>[Cl:1][C:2]1[CH:7]=[C:6]([NH:11][NH2:12])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1

참가 물질

4

반응물 2

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

생성물 1

HCID 14845464-Chloro-6-hydrazinyl-2-(methylsulfanyl)pyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

33 g (169.2 mmol) of 4,6-dichloro-2-(methylthio)pyrimidine are introduced into 300 ml of THF at −20° C., and 169 ml of a 1M solution of hydrazine in THF is added dropwise at a rate such that the temperature does not rise above −15° C. The mixture is stirred at 0° C. for a further 2 h. After the reaction is complete, the solvent is distilled off and the residue is stirred with diethyl ether. 18.4 g (57% of theory) of the product are obtained as a solid.

후처리

  1. customdoes not rise above −15° C
  2. distillationthe solvent is distilled off
  3. stirringthe residue is stirred with diethyl ether
  4. custom18.4 g (57% of theory) of the product are obtained as a solid

출처 및 근거

ORD 기록
ord-5eaf8aeddcf1430d8ea9d2394de1b059
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273752B2

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