RU 25591 → HCID 21153170, 화합물

HRID 1447650노트

반응식

HRID 1447650 반응식
[CH3:1][N:2]([CH3:24])[C@@H:3]1[CH2:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[C@H:5]([O:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][CH:16]=2)[CH2:4]1>C(O)C.[H][H].[Pt](=O)=O>[CH3:1][N:2]([CH3:24])[C@@H:3]1[CH2:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[C@H:5]([O:14][C:15]2[CH:16]=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=2)[CH2:4]1

참가 물질

5

반응물 1

HCID 182578RU 25591

생성물 1

HCID 21153170HCID 21153170, 화합물수율 107.1%

시약·촉매·용매 3

HCID 345198Adams' catalyst촉매HCID 702Ethanol용매HCID 178418361HCID 178418361, 화합물용매

실험 절차

370 mg of platinum dioxide were added to a solution of 3.7 g of cis N,N-dimethyl-5-[4-nitrophenoxy]-6,7,8,9-tetrahydro-benzocycloheptene-7-amine in 200 ml of ethanol and one liter of hydrogen was bubbled therethrough for 30 minutes with stirring. The mixture was filtered and the filtrate was evaporated to dryness under reduced pressure to obtain 3.6 g of cis N,N-dimethyl-5-[4-aminophenoxy]-6,7,8,9-tetrahydro-5H-benzocycloheptene-7-amine in the form of an orange oil. The said oil was dissolved in 20 ml of ethyl acetate and a solution of ethyl acetate saturated with gaseous hydrogen chloride was added thereto to adjust the pH to 1. The mixture stood for one hour at room temperature and was then vacuum filtered to obtain 4.1 g of the dihydrochloride of the cis compound in the form of colorless crystals melting at ≈260° C.

후처리

  1. customwas bubbled
  2. filtrationThe mixture was filtered
  3. customthe filtrate was evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-d72f181dd1b04766b1328306636529e8
출처 데이터셋
uspto-grants-1979_12
특허 번호
US04177292

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