반응식
[NH:1]([C:5]1[C:13]([N+:14]([O-:16])=[O:15])=[CH:12][C:8]2[O:9][CH2:10][O:11][C:7]=2[CH:6]=1)C(C)=O.C[O-].[Na+].C(O)(=O)C>CO>[NH2:1][C:5]1[C:13]([N+:14]([O-:16])=[O:15])=[CH:12][C:8]2[O:9][CH2:10][O:11][C:7]=2[CH:6]=1참가 물질
실험 절차
40 g of 5-acetamino-6-nitro-1,3-benzodioxole were dissolved with heating in 4 l of methanol in a 10 l round flask equipped with a reflux condenser. To this hot solution was added a boiling solution of 40 g of sodium methoxide in 4 l of methanol and the mixture was boiled under reflux for exactly 15 minutes. Then, the reaction was interrupted by adding 220 ml of glacial acetic acid. The methanol was removed by distillation and the last traces thereof, together with the glacial acetic acid, were removed by a two-fold evaporation with toluene. The product went into solution with 3 l of methylene chloride and could be freed from the organic residues by suction filtration. The methylene chloride solution was filtered through silicon dioxide and evaporated in vacuo. The residue, recrystallized from isopropanol, gave 30.9 g (95% of theory) of 5-amino-6-nitro-1,3-benzodioxole of melting point 203°-204° C.
후처리
- customequipped with a reflux condenser
- temperatureunder reflux for exactly 15 minutes
- customThe methanol was removed by distillation
- customthe last traces thereof, together with the glacial acetic acid, were removed by a two-fold evaporation with toluene
- filtrationcould be freed from the organic residues by suction filtration
- filtrationThe methylene chloride solution was filtered through silicon dioxide
- customevaporated in vacuo
- customThe residue, recrystallized from isopropanol
출처 및 근거
- ORD 기록
- ord-5db1c651cb40476093ba6515ba0ec03a
- 출처 데이터셋
- uspto-grants-1986_07
- 특허 번호
- US04599347
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