Ammonium Chloride → 4-Cyclopropylbenzene-1,2-diamine
반응식
[CH:1]1([C:4]2[CH:10]=[CH:9][C:7]([NH2:8])=[C:6]([N+:11]([O-])=O)[CH:5]=2)[CH2:3][CH2:2]1.[Cl-].[NH4+]>CO.[Zn]>[CH:1]1([C:4]2[CH:5]=[C:6]([NH2:11])[C:7]([NH2:8])=[CH:9][CH:10]=2)[CH2:3][CH2:2]1참가 물질
5
실험 절차
4-Cyclopropyl-2-nitroaniline (178 mg, 1 mmol) was dissolved in absolute methanol (6 mL), and zinc powder (200 mg, 3.1 mmol) and ammonium chloride (800 mg, 15 mmol) were added. The mixture was stirred at room temperature for 16 hours. The mixture was filtered through a pad of celite, and the filtrate was concentrated in vacuo. The residue was partitioned between water (30 mL) and dichloromethane (30 mL). The organic layer was separated, and the aqueous layer was extracted twice with dichloromethane (15 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo to give 4-cyclopropyl-benzene-1,2-diamine as a brown solid which was used without further purification (130 mg, 88%).
후처리
- filtrationThe mixture was filtered through a pad of celite
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was partitioned between water (30 mL) and dichloromethane (30 mL)
- customThe organic layer was separated
- extractionthe aqueous layer was extracted twice with dichloromethane (15 mL)
- dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-f28116a9b5b7412f9bea78a9b8681c92
- 출처 데이터셋
- uspto-grants-2009_07
- 특허 번호
- US07557221B2
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