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

HRID 234835노트

반응식

HRID 234835 반응식
[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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
40 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9e1bfebc22bf4f6f8c0d98280c2d7cb8
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596097

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