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

HRID 330446

反応式

HRID 330446 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 142756782-Isothiocyanato-4-methoxy-6-methylpyrimidine収率 63.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-09ed0ef466724d298214983b1f0b370d
出典データセット
uspto-grants-1990_01
特許番号
US04897105

関連ノート

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