반응식
O.O.[Sn](Cl)Cl.[N:6]1([C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[C:14]([N+:20]([O-])=O)[CH:13]=2)[CH2:11][CH2:10][O:9][CH2:8][CH2:7]1.[OH-].[Na+]>Cl>[NH2:20][C:14]1[CH:13]=[C:12]([N:6]2[CH2:7][CH2:8][O:9][CH2:10][CH2:11]2)[CH:19]=[CH:18][C:15]=1[C:16]#[N:17]참가 물질
5
실험 절차
To a cooled mixture of tin(II) chloride dihydrate 12.8 g (56.7 mmol) in conc. HCl mL with ice bath was added 4-(morpholin-4-yl)-2-nitrobenzonitrile 4.20 g (16.09 mmol) and stirred at room temperature for 2 hours. The reaction mixture was poured into diluted NaOH solution and extracted into ethyl acetate. The organic layer was washed with water and brine, dried over MgSO4 and the solvent was evaporated. The crude product was washed with diethyl ether to give the title compound 3.13 g as off-white solid. Yield 95.0%.
후처리
- extractionextracted into ethyl acetate
- washThe organic layer was washed with water and brine
- dry with materialdried over MgSO4
- customthe solvent was evaporated
- washThe crude product was washed with diethyl ether
출처 및 근거
- ORD 기록
- ord-21ef5eb7f24949b289e1ca76d8b6b19d
- 출처 데이터셋
- uspto-grants-2012_03
- 특허 번호
- US08129386B2
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