Hydrogen chloride-ethyl acetate → (6r)-6-(Methoxymethyl)-3-[2-(methoxymethyl)pyrrolidin-1-yl]-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine hydrochloride
반응식
C([N:8]1[CH2:14][C:13]2[N:15]=[CH:16][C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][O:25][CH3:26])=[N:18][C:12]=2[O:11][C@@H:10]([CH2:27][O:28][CH3:29])[CH2:9]1)C1C=CC=CC=1.C(OCC)(=O)C.[ClH:36]>CO.[OH-].[OH-].[Pd+2]>[ClH:36].[CH3:29][O:28][CH2:27][C@H:10]1[CH2:9][NH:8][CH2:14][C:13]2[N:15]=[CH:16][C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][O:25][CH3:26])=[N:18][C:12]=2[O:11]1참가 물질
5
반응물 2
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 50 °C
실험 절차
To a solution of (6R)-8-benzyl-6-(methoxymethyl)-3-[2-(methoxymethyl)pyrrolidin-1-yl]-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine (329 mg) in methanol (10 mL) was added 20% Pd(OH)2/C (40 mg), and the mixture was stirred under a hydrogen atmosphere at 50° C. for 3 hr. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. To a solution of the obtained crude product in ethyl acetate (10 mL) was added a 4 N hydrogen chloride-ethyl acetate solution (227 μL), and the mixture was stirred for 30 min. The reaction mixture was filtered, and the obtained crystals were washed with ethyl acetate to give the title compound (155 mg, 54%).
후처리
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure
- customTo a solution of the obtained crude product in ethyl acetate (10 mL)
- stirringthe mixture was stirred for 30 min
- filtrationThe reaction mixture was filtered
- washthe obtained crystals were washed with ethyl acetate
출처 및 근거
- ORD 기록
- ord-80e8ef11036e4130b01b5d727c103832
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08314088B2
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