m-Chloroperbenzoic acid → 4-Chloro-2,6-dimethylpyrimidine 1-oxide

HRID 1755651노트

반응식

HRID 1755651 반응식
[CH3:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.ClC1C=CC=C(C(OO)=[O:18])C=1>ClCCl>[CH3:1][C:2]1[N+:7]([O-:18])=[C:6]([CH3:8])[CH:5]=[C:4]([Cl:9])[N:3]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 31541994-Chloro-2,6-dimethylpyrimidine

생성물 1

HCID 126992254-Chloro-2,6-dimethylpyrimidine 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
5 °C

실험 절차

20 g (14.03×10-2 mol) of 2,4-dimethyl-6-chloropyrimidine are dissolved in 300 ml of dichloromethane in a 500 ml three-necked flask fitted with a thermometer and a magnetic stirrer. The mixture is cooled to 5° C. and 65.3 g of 55% metachloroperbenzoic acid, which is about 1.5 equivalents, are then added in solid portions. The reaction mixture is then stirred for 24 hours at ambient temperature (25° C.) and then filtered through a 3 frit. The filtrate is washed with 150 ml of a 6% aqueous sodium hydroxide solution and then with 2×50 ml of water to render neutral. It is then dried over sodium sulphate and then filtered through paper and evaporated. The crude mass is recrystallised from n-hexane.

후처리

  1. customfitted with a thermometer and a magnetic stirrer
  2. additionare then added in solid portions
  3. filtrationfiltered through a 3 frit
  4. washThe filtrate is washed with 150 ml of a 6% aqueous sodium hydroxide solution
  5. dry with materialIt is then dried over sodium sulphate
  6. filtrationfiltered through paper
  7. customevaporated
  8. customThe crude mass is recrystallised from n-hexane

출처 및 근거

ORD 기록
ord-8eb253211e7e4ba6b81072fad965b435
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05438058

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