Hydrochloric Acid → (S)-4,4-Dimethylpyrrolidin-3-OL hydrochloride
반응식
[CH3:1][C:2]1([CH3:15])[CH2:6][N:5](CC2C=CC=CC=2)[CH2:4][C@H:3]1[OH:14].[ClH:16]>CO.[Pd]>[ClH:16].[CH3:1][C:2]1([CH3:15])[CH2:6][NH:5][CH2:4][C@H:3]1[OH:14]참가 물질
5
실험 절차
To a solution of (3S)-4,4-dimethyl-1-(phenylmethyl)-3-pyrrolidinol (J. Med. Chem. 1992, 35, 4205-4213) (0.7738 g, 3.769 mmol) in MeOH (38 mL) was added 1 N aq. HCl (3.8 mL, 3.8 mmol) and 10% Pd/C (50% water, 230 mg). The mixture was hydrogenated under balloon pressure for 18 h, and was then filtered through a 0.2 μm filter tip syringe. The resulting solution was concentrated in vacuo and azeotroped with MeOH (2×50 mL) to afford (3S)-4,4-dimethyl-3-pyrrolidinol hydrochloride (0.5267 g, 93% yield) as a light orange solid. LCMS: (M+H)+: 116.1.
후처리
- filtrationwas then filtered through a 0.2 μm
- filtrationfilter tip syringe
- concentrationThe resulting solution was concentrated in vacuo
- customazeotroped with MeOH (2×50 mL)
출처 및 근거
- ORD 기록
- ord-5fab1a010159469ba2d530377a997467
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07893056B2
반응 노트
불러오는 중…