Ammonia → alpha-Amino-1,3-benzodioxole-5-acetonitrile
반응식
[CH:1]1[C:6]([CH:7]=O)=[CH:5][C:4]2[O:9][CH2:10][O:11][C:3]=2[CH:2]=1.[NH3:12].[NH4+:13].[Cl-].[C-:15]#N.[K+].[O-]S([O-])(=O)=O.[Mg+2]>C1COCC1>[NH2:12][CH:7]([C:6]1[CH:1]=[CH:2][C:3]2[O:11][CH2:10][O:9][C:4]=2[CH:5]=1)[C:15]#[N:13]참가 물질
7
실험 절차
Piperonal (6.00 g) is dissolved in THF (25 mL) and aq. NH3 (58%, 4.2 mL), NH4Cl (3.3 g) and KCN (3.9 g) are added. The mixture is stirred efficiently for 24 h. MgSO4 is added and the mixture stirred for 30 min., filtered and washed with THF. The filtrate is evaporated under reduced pressure and the residue purified by FC (Et2O/petrol ether 1:2,→2:1,→Et2O). Aminonitrile W-99 is obtained as a brown, unstable oil (2.87 g). The hydrochloride salt is precipitated from sat. HCl/Et2O for analytical purposes.
후처리
- stirringthe mixture stirred for 30 min.
- filtrationfiltered
- washwashed with THF
- customThe filtrate is evaporated under reduced pressure
- customthe residue purified by FC (Et2O/petrol ether 1:2,→2:1,→Et2O)
출처 및 근거
- ORD 기록
- ord-6f3872981ba44ed0a4dc05cc01bc6b5d
- 출처 데이터셋
- uspto-grants-2001_04
- 특허 번호
- US06211376B1
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