Hexamethylenetetramine → 4,4-Dimethoxy-2-methylbut-2-enal
반응식
Br[CH2:2][CH:3]=[C:4](C)[CH:5]([O:8][CH3:9])[O:6][CH3:7].C1N2CN3CN(C2)CN1C3.[Cl-].[Na+].[CH:23]([O:26]C(C)C)(C)C>O>[CH3:9][O:8][CH:5]([O:6][CH3:7])[CH:4]=[C:3]([CH3:2])[CH:23]=[O:26]참가 물질
6
실험 절차
4-Bromo-1,1-dimethoxy-2-methyl-2-butene (2 g) was added to a solution of hexamine (1.7 g) and water (10 ml), and the mixture was stirred at room temperature for 14 hours. Dowex 50×8 (type H)(3 g) was previously treated with sodium chloride to convert it to type Na. Then isopropyl ether (20 ml) was added to the above reaction mixture, the type Na resin was added, and the mixture was stirred at 70° C. for 6 hours. The isopropyl ether layer was separated, concentrated and purified by column chromatography to give 4,4-dimethoxy-2-methyl-2-buten-1-al (0.92 g, 64%).
후처리
- additionthe type Na resin was added
- stirringthe mixture was stirred at 70° C. for 6 hours
- customThe isopropyl ether layer was separated
- concentrationconcentrated
- custompurified by column chromatography
출처 및 근거
- ORD 기록
- ord-14c9aad48624413d905738f079d73073
- 출처 데이터셋
- uspto-grants-1995_11
- 특허 번호
- US05471004
반응 노트
불러오는 중…