RU 25591 → HCID 21153170、化合物

HRID 1447650ノート

反応式

HRID 1447650 の反応式
[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

参加物

5

反応物 1

HCID 182578RU 25591

生成物 1

HCID 21153170HCID 21153170、化合物収率 107.1%

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d72f181dd1b04766b1328306636529e8
出典データセット
uspto-grants-1979_12
特許番号
US04177292

反応ノート

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