Water → 1-Naphthylamine

HRID 541169

반응식

HRID 541169 반응식
[N+:1]([C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1)([O-])=O.O>C(OCC)(=O)C>[NH2:1][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 68491-Nitronaphthalene

생성물 1

HCID 86401-Naphthylamine수율 62%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

86.6 mg (0.50 mmol) of 1-nitronaphthalene (17), 270 μL (15 mmol) of distilled water and stainless steel balls (50 pieces) were placed in the vessel of the planetary ball mill, which was then closed, and agitated by operating the planetary ball mill for 12 hours at 800 rpm (reversed every 30 minutes). After the lapse of 12 hours, 10 mL of ethyl acetate was added to the vessel of the planetary ball mill to provide a solution containing the reaction mixture, which was then filtered with celite. The operation was repeated 5 times to provide a filtrate, which was then concentrated, thereby providing 44.3 mg (0.31 mmol) of 1-aminonaphthalene (18). The yield was 62%. The conversion yield was 100%, but the isolated yield was lowered since the product was partially distilled off under reduced pressure. The reaction is expressed by the following scheme.

후처리

  1. customwas then closed
  2. customfor 12 hours
  3. customto provide a solution
  4. additioncontaining the reaction mixture, which
  5. filtrationwas then filtered with celite
  6. customto provide a filtrate, which
  7. concentrationwas then concentrated

출처 및 근거

ORD 기록
ord-6ce55f82bdaa4c479184c2720db64d59
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871980B2

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