N-bromobutanimide → 3-Bromo-5,7-dichloropyrazolo[1,5-a]pyrimidine
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]2[N:9]=[CH:10][CH:11]=[C:4]2[N:3]=1.[Br:12]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Br:12][C:11]1[CH:10]=[N:9][N:5]2[C:6]([Cl:8])=[CH:7][C:2]([Cl:1])=[N:3][C:4]=12参加物
4
実験手順
To a solution of 5.3 g of 5,7-dichloropyrazolo(1,5-a)pyrimidine in 70 ml of chloroform was added portionwise 6 g of N-bromosuccinimide while keeping the temperature below 40° C. The resulting solution was refluxed for 30 minutes and was then stirred at room temperature for 12 hours. The suspension was then filtered. The filtrate was washed with 50 ml of cold 10% sodium hydroxide aqueous solution twice and was then dried over MgSO4. The chloroform solution was then concentrated under reduced pressure to give 7.47 g of the desired product, m.p. 73°-75° C.
後処理
- customthe temperature below 40° C
- temperatureThe resulting solution was refluxed for 30 minutes
- filtrationThe suspension was then filtered
- washThe filtrate was washed with 50 ml of cold 10% sodium hydroxide aqueous solution twice
- dry with materialwas then dried over MgSO4
- concentrationThe chloroform solution was then concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0490b71736b148aa95b88f2051841249
- 出典データセット
- uspto-grants-1989_06
- 特許番号
- US04838925
反応ノート
読み込み中…