Hydrochloric Acid → 4-(Azetidin-3-yl)morpholine dihydrochloride
반응식
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:9]2)C=CC=CC=1.[ClH:24]>[OH-].[Pd+2].[OH-].C(O)C>[ClH:24].[ClH:24].[O:15]1[CH2:16][CH2:17][N:12]([CH:10]2[CH2:11][NH:8][CH2:9]2)[CH2:13][CH2:14]1참가 물질
5
실험 절차
A mixture of 1-diphenylmethyl-3-morpholinoazetidine (see PREPARATION 12) (18.6 g, 60.4 mmol), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous hydrochloric acid solution (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50 p.s.i.) for three days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration yielded a solid which was recrystallised from methanol to give the title compound (10.2 g) as a crystalline solid.
후처리
- customThe catalyst was then removed by filtration
- customthe filtrate evaporated to dryness
- additionAddition of dichloromethane (100 ml) to the residue and trituration
- customyielded a solid which
- customwas recrystallised from methanol
출처 및 근거
- ORD 기록
- ord-ac252939b8064dddbbb807dbbd727aa5
- 출처 데이터셋
- uspto-grants-2001_06
- 특허 번호
- US06242438B1
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