Hydrochloric Acid → 2-[2-(amino)ethyl]-5-[[2-(amino)ethyl]amino]isoquino[8,7,6-cd]indazole-6(2H)-one trihydrochloride

HRID 234835ノート

反応式

HRID 234835 の反応式
[ClH:1].C(OC([NH:9][CH2:10][CH2:11][N:12]1[C:20]2[CH:19]=[CH:18][C:17]([NH:21][CH2:22][CH2:23][NH:24]C(OC(C)(C)C)=O)=[C:16]3[C:32](=[O:39])[C:33]4[CH:34]=[CH:35][N:36]=[CH:37][C:38]=4[C:14]([C:15]=23)=[N:13]1)=O)(C)(C)C>C(O)C>[ClH:1].[ClH:1].[ClH:1].[NH2:9][CH2:10][CH2:11][N:12]1[C:20]2[CH:19]=[CH:18][C:17]([NH:21][CH2:22][CH2:23][NH2:24])=[C:16]3[C:32](=[O:39])[C:33]4[CH:34]=[CH:35][N:36]=[CH:37][C:38]=4[C:14]([C:15]=23)=[N:13]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 108158792-[2-(N-tert-butoxycarbonylamino)ethyl]-5-[[2-(N-tert-butoxycarbonylamino)ethyl]amino]isoquino[8,7,6-cd]indazole-6(2H)-one

生成物 1

HCID 199747312-[2-(amino)ethyl]-5-[[2-(amino)ethyl]amino]isoquino[8,7,6-cd]indazole-6(2H)-one trihydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

Under a nitrogen atmosphere an ethanolic solution of anhydrous HCl (5N; 0.40 mL) is dropped into a stirred suspension of 2-[2-(N-tert-butoxycarbonylamino) ethyl]-5-[[2-(N-tert-butoxycarbonylamino) ethyl]amino]isoquino[8,7,6-cd]indazole-6(2H)-one of Example 20 (0.104 g) in absolute ethanol (2.1 mL). Initial dissolution of the starting material followed by precipitation of a dark-red solid is observed during the addition of ethanolic HCI. This solid is redissolved with absolute ethanol and the solution is heated to 40° C. for 2 h, 30'. The gradual formation of a redamaranth precipitate is observed during the heating. After cooling to room temperature diethyl ether (10 mL) is added and the precipitate is collected by suction filtration under a nitrogen blanket, to give 2-[2-(amino)ethyl]-5-[[2-(amino)ethyl]amino]isoquino[8,7,6-cd]indazole-6(2H)-one trihydrochloride (0.070 g).

後処理

  1. dissolutionInitial dissolution of the starting material
  2. customfollowed by precipitation of a dark-red solid
  3. additionis observed during the addition of ethanolic HCI
  4. dissolutionThis solid is redissolved with absolute ethanol
  5. temperatureAfter cooling to room temperature diethyl ether (10 mL)
  6. additionis added
  7. filtrationthe precipitate is collected by suction filtration under a nitrogen blanket

出典と根拠

ORDレコード
ord-9e1bfebc22bf4f6f8c0d98280c2d7cb8
出典データセット
uspto-grants-1997_01
特許番号
US05596097

反応ノート

読み込み中…