1,3-Dibromopropane → HCID 54351699, 화합물
반응식
C(=O)([O-])[O-].[K+].[K+].[CH3:7][C:8]1[CH:9]=[C:10]([CH:24]=[C:25]([CH3:28])[C:26]=1[OH:27])[C:11]([C:13]1[O:14][C:15]2[C:20]([C:21](=[O:23])[CH:22]=1)=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:12].[Br:29][CH2:30][CH2:31][CH2:32]Br>CN(C)C=O>[Br:29][CH2:30][CH2:31][CH2:32][O:27][C:26]1[C:25]([CH3:28])=[CH:24][C:10]([C:11]([C:13]2[O:14][C:15]3[C:20]([C:21](=[O:23])[CH:22]=2)=[CH:19][CH:18]=[CH:17][CH:16]=3)=[O:12])=[CH:9][C:8]=1[CH3:7]참가 물질
5
실험 절차
27.6 g (0.2 mol) of potassium carbonate was added to a solution of 29.4 g (0.1 mol) of 2-(3,5-dimethyl 4-hydroxy benzoyl) chromone in 150 ml of dimethyl formamide, 101 g (0.5 mol) of 1,3-dibromo propane was added and the admixture left at ambient temperature for 15 hours with constant agitation. The potassium bromide precipitate was filtered, the dimethyl formamide was concentrated in vacuo and the residue dissolved in 300 ml of water. Extraction was effected with 200 ml of methylene chloride, and precipitation was then effected by adding 200 ml of ether. The product was 36 g of 2-[4-(3-bromo propoxy) 3,5-dimethyl benzoyl] chromone.
후처리
- additionwas added
- filtrationThe potassium bromide precipitate was filtered
- concentrationthe dimethyl formamide was concentrated in vacuo
- dissolutionthe residue dissolved in 300 ml of water
- extractionExtraction
- customwas effected with 200 ml of methylene chloride, and precipitation
- additionby adding 200 ml of ether
출처 및 근거
- ORD 기록
- ord-27d8c0d2087641c8b0183c2e60b2269a
- 출처 데이터셋
- uspto-grants-1980_09
- 특허 번호
- US04220645
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