Phenyl thioxochloroformate → 2-Isothiocyanato-4-methoxy-6-methylpyrimidine

HRID 330446

반응식

HRID 330446 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[N:6]=[C:5]([NH:10][Si](C)(C)C)[N:4]=1.C1C=CC(O[C:22](Cl)=[S:23])=CC=1>C1(C)C=CC=CC=1>[N:10]([C:5]1[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([CH3:9])[N:6]=1)=[C:22]=[S:23]

참가 물질

4

반응물 2

HCID 70498Phenyl thioxochloroformateHCID 135876394-Methoxy-6-methyl2-trimethylsilylaminopyrimidine

생성물 1

HCID 142756782-Isothiocyanato-4-methoxy-6-methylpyrimidine수율 63.9%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

A mixture of 4.2 g of 4-methoxy-6-methyl-2-trimethylsilylaminopyrimidine and 3.5 g of phenyl chlorothionocarbonate in 30 ml of toluene is stirred with heating at ca. 80° C. for 5.5 hours. The reaction solution is cooled to room temperature and filtered to remove the precipitate. The filtrate is concentrated under reduced pressure, and the residue is purified by silica gel chromatography (eluent: ethyl acetate: toluene =1:3) to give the title compound (2.3 g). mp 54°~55° C.

후처리

  1. temperatureThe reaction solution is cooled to room temperature
  2. filtrationfiltered
  3. customto remove the precipitate
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customthe residue is purified by silica gel chromatography (eluent: ethyl acetate: toluene =1:3)

출처 및 근거

ORD 기록
ord-09ed0ef466724d298214983b1f0b370d
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04897105

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