Phosphorus oxychloride → 2-Chloro-4,6-dimethyl-5-nitropyrimidine

HRID 2046309노트

반응식

HRID 2046309 반응식
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[N:5]=[C:4](O)[N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:4]1[N:3]=[C:2]([CH3:1])[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[N:5]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178433502HCID 178433502, 화합물

생성물 1

HCID 593361732-Chloro-4,6-dimethyl-5-nitropyrimidine수율 74.1%

실험 절차

A mixture of Compound 1 (500 mg) and phosphorus oxychloride (3.89 g) was stirred for 3 hours under reflux. After the reaction was completed, the mixture was concentrated under reduced pressure. To the resulting residue, chloroform and water were added and the mixture was cooled and neutralized with a 2N aqueous sodium hydroxide solution to a pH of 5 to 7. The mixture was then extracted with chloroform and the organic layer was concentrated under reduced pressure to obtain 411 mg of the desired product. When necessary, some of the product was purified by silica gel column chromatography (ethyl acetate:hexane=1:1) to give a purified product.

후처리

  1. temperatureunder reflux
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionTo the resulting residue, chloroform and water were added
  4. temperaturethe mixture was cooled
  5. extractionThe mixture was then extracted with chloroform
  6. concentrationthe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ddc622b86f36401fb4eabe652680dd57
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592435B2

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