Water → (5,5-Dimethyloxolan-2-yl)methanamine
반응식
[N:1]([CH2:4][CH:5]1[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][CH2:6]1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O>C1COCC1>[CH3:10][C:8]1([CH3:11])[O:9][CH:5]([CH2:4][NH2:1])[CH2:6][CH2:7]1참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
5-(Azidomethyl)-2,2-dimethyltetrahydrofuran (22 g, 142 mmol) in THF (500 ml) was treated with Triphenylphosphine (39.0 g, 149 mmol) and t stirred for 5 mins. Water (50.0 ml) was added and the reaction mixture was heated at 80° C. for 4 hrs. The mixture was passed through Isolute® SCX-2 resin (200 g 0.67 mmol/g) eluting with MeOH (500 ml), DMSO (100 ml), 20% MeOH:DCM (500 ml), MeOH (500 ml) followed 7M ammonia in MeOH (500 ml). The ammonia layer was evaporated to dryness to afford the title compound.
후처리
- washeluting with MeOH (500 ml), DMSO (100 ml), 20% MeOH
- customThe ammonia layer was evaporated to dryness
출처 및 근거
- ORD 기록
- ord-2cf5a4f17b3a457a928f2591c5ae192c
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08883819B2
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