Acetic Anhydride → HCID 12838038, 화합물
반응식
Cl.[Cl:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[CH2:11][NH:10][CH2:9][CH2:8]2.[OH-].[Na+].C([O-])(O)=O.[Na+].[C:20](OC(=O)C)(=[O:22])[CH3:21]>ClCCl>[C:20]([N:10]1[CH2:9][CH2:8][C:7]2[C:12](=[C:3]([Cl:2])[CH:4]=[CH:5][CH:6]=2)[CH2:11]1)(=[O:22])[CH3:21]참가 물질
6
실험 절차
To a mixture of 28.6 g of 8-chloro-1,2,3,4-tetrahydoisoquinoline hydrochloride in 140 ml of dichloromethane was added 140 ml of 1N aqueous NaOH solution and 17.6 g of NaHCO3. To the solution was added dropwise 14.5 ml of acetic anhydride at 5° C. The mixture was stirred at room temperature for 1 hour. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic extracts were washed with water, dried over anhydrous sodium sulfate. The solvent was distilled off to give 29.1 g of the title compound as a pale red oil.
후처리
- customThe organic layer was separated
- extractionthe aqueous layer was extracted with dichloromethane
- washThe combined organic extracts were washed with water
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off
출처 및 근거
- ORD 기록
- ord-95ad5da48c2b4f3eac985c169b57df40
- 출처 데이터셋
- uspto-grants-1993_12
- 특허 번호
- US05273974
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