Government regulation → HCID 14125892,化合物
反应方程式
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]([CH2:15][CH2:16][CH2:17][Cl:18])=[O:14])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:19]Br>C(O)(=O)C>[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]([CH:15]([Br:19])[CH2:16][CH2:17][Cl:18])=[O:14])=[CH:9][CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1参与物
4
实验过程
246 g (0.95 mol) of 3-chloropropyl 4-phenylphenyl ketone in 380 ml of glacial acetic acid were placed in a reaction flask and 152 g (0.95 mol) of bromine were added dropwise at 30° C., the reaction commencing with dissolution and decolorization. After 1 hour, a thick precipitate deposited. The mixture was stirred for a further 4 hours at room temperature in order to complete the reaction. The crystals produced were filtered off under suction, washed with water, dissolved in dichloromethane, washed by shaking with NaHCO3 solution and water and dried, and 250 g (78% of theory) of the title substance were obtained as colorless crystals of melting point 85°-88° C.
后处理
- dissolutionthe reaction commencing with dissolution and decolorization
- customthe reaction
- customThe crystals produced
- filtrationwere filtered off under suction
- washwashed with water
- dissolutiondissolved in dichloromethane
- washwashed
- stirringby shaking with NaHCO3 solution and water
- customdried
- custom250 g (78% of theory) of the title substance were obtained as colorless crystals of melting point 85°-88° C.
来源与证据
- ORD记录
- ord-8667b01de8eb4dc28a469c06b315aa42
- 来源数据集
- uspto-grants-1989_05
- 专利号
- US04829075
反应笔记
加载中…