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HCID 20094804, 화합물 → 3-methoxy-6,7,8,9-tetrahydro-5H-benzo[7]annulen-6-amine

HRID 274073
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인쇄 미리보기

반응식

HRID 274073 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:12](=O)[CH2:11][CH2:10][CH:9]([N+:14]([O-])=O)[CH2:8][C:7]=2[CH:17]=1.[H][H]>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][CH:9]([NH2:14])[CH2:8][C:7]=2[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 20094804HCID 20094804, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 180073203-methoxy-6,7,8,9-tetrahydro-5H-benzo[7]annulen-6-amine수율 94.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

A solution of 2-methoxy-8-nitro-6,7,8,9-tetrahydro-5H-benzocyclohepten-5-one (0.20 g) in acetic acid (2 ml) was hydrogenated at 4 atm hydrogen atmosphere over 10% palladium on carbon (0.20 g). After removing the catalyst, the pH of the solution was adjusted to 12 with sodium hydroxide solution and the solution was extracted with ethyl acetate. The extract was washed with brine, dried over potassium carbonate, and evaporated in vacuo to give 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-amine (153 mg).

후처리

  1. customAfter removing the catalyst
  2. extractionthe solution was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over potassium carbonate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-4da40cfde7f443c5bfd2239d4256aa10
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05387710

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