N-bromobutanimide → HCID 20514104、化合物

HRID 1902884ノート

反応式

HRID 1902884 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 20514104HCID 20514104、化合物収率 75.1%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2f02c1f727054850a10c993fb209e740
出典データセット
uspto-grants-1982_12
特許番号
US04366189

反応ノート

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