Ammonium Chloride → 4-Cyclopropylbenzene-1,2-diamine

HRID 227161노트

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HRID 227161 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]1

참가 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

  1. filtrationThe mixture was filtered through a pad of celite
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was partitioned between water (30 mL) and dichloromethane (30 mL)
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted twice with dichloromethane (15 mL)
  6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f28116a9b5b7412f9bea78a9b8681c92
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557221B2

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