N-bromobutanimide → HCID 20514104, 화합물

HRID 1902884노트

반응식

HRID 1902884 반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[CH:16]=[C:15]([CH3:17])[N:14]=[C:13]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)[N:12]=1>ClC(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:1][CH2:24][C:21]1[CH:22]=[CH:23][C:18]([C:13]2[N:12]=[C:11]([O:10][CH3:9])[CH:16]=[C:15]([CH3:17])[N:14]=2)=[CH:19][CH:20]=1

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 205140954-Methoxy-6-methyl-2-(4-methylphenyl)pyrimidine

생성물 1

HCID 20514104HCID 20514104, 화합물수율 75.1%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride용매

실험 절차

A mixture of 9.4 g of N-bromosuccinimide and 0.2 g of azoisobutyronitrile is added in portions at 70° C. and in the course of 30 minutes to a solution of 10.7 g of 4-methoxy-6-methyl-2-p-tolylpyrimidine and 0.2 g of dibenzoyl peroxide in 100 ml of anhydrous tetrachloromethane. The mixture is then kept for 2 hours at reflux temperature. After cooling, the succinimide is filtered with suction and the filter cake is washed with 200 ml of tetrachloromethane and the filtrate is concentrated. Recrystallisation from n-hexane affords 11 g (75% of theory) of 2-(4-bromomethylphenyl)-4-methoxy-6-methylpyrimidine with a melting point of 98°-99° C.

후처리

  1. temperatureat reflux temperature
  2. temperatureAfter cooling
  3. filtrationthe succinimide is filtered with suction
  4. washthe filter cake is washed with 200 ml of tetrachloromethane
  5. concentrationthe filtrate is concentrated
  6. customRecrystallisation from n-hexane

출처 및 근거

ORD 기록
ord-2f02c1f727054850a10c993fb209e740
출처 데이터셋
uspto-grants-1982_12
특허 번호
US04366189

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