反応式
P(Br)(Br)[Br:2].OC1[C:7]([C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[CH:21]=2)=[N:8][CH:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:10](C)C=1C.C(=O)([O-])[O-].[K+].[K+].O1[CH2:39][CH2:38][CH2:37][CH2:36]1>C1C=CC=CC=1>[Br:2][CH2:36][C:37]1[C:7]([C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[CH:21]=2)=[N:8][C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:10][C:38]=1[CH3:39]参加物
実験手順
To a solution of phosphorus tribromide (16.85 g) in a mixture of benzene (150 ml) and tetrahydrofuran (150 ml) was dropwise added a solution of 5-hydroxy-methyl-6-methyl-2-phenyl-4-(3-nitrophenyl)pyrimidine (30 g) in tetrahydrofuran (150 ml) under cooling at 7°-10° C. After stirring for 4 hours at the same temperature, the reaction mixture was poured into ice-water (200 ml), adjusted to pH 9.5 with saturated potassium carbonate and extracted with ethyl acetate (300 ml). After filtering off an insolble material, the organic layer was washed with saturated aqueous sodium chloride, dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from diethyl ether to give 5-bromomethyl-6-methyl-2-phenyl-4-(3-nitrophenyl)pyrimidine (29.08 g).
後処理
- temperatureunder cooling at 7°-10° C
- extractionextracted with ethyl acetate (300 ml)
- filtrationAfter filtering off an insolble material
- washthe organic layer was washed with saturated aqueous sodium chloride
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was recrystallized from diethyl ether
出典と根拠
- ORDレコード
- ord-5445957897b14e47a375be80f7ca2538
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04727073
関連ノート
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