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Hydrochloric Acid → HCID 21874036, 화합물

HRID 729241
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HRID 729241 반응식
[ClH:1].O1CCOCC1.[CH3:8][N:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:43]=[CH:42][C:18]([C:19]([NH:21][C:22]3[C:23]4[CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][C:24]=4[N:25]([C:27]([O:29][CH2:30][CH3:31])=[O:28])[N:26]=3)=[O:20])=[CH:17][CH:16]=2)[CH2:11][CH2:10]1>C(Cl)Cl>[ClH:1].[ClH:1].[ClH:1].[CH3:8][N:9]1[CH2:10][CH2:11][N:12]([C:15]2[CH:43]=[CH:42][C:18]([C:19]([NH:21][C:22]3[C:23]4[CH2:34][NH:33][CH2:32][C:24]=4[N:25]([C:27]([O:29][CH2:30][CH3:31])=[O:28])[N:26]=3)=[O:20])=[CH:17][CH:16]=2)[CH2:13][CH2:14]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 112373285-tert-Butyl 1-ethyl 3-[4-(4-methylpiperazin-1-yl)benzamido]-4,6-dihydropyrrolo[3,4-c]pyrazole-1,5-dicarboxylate

생성물 1

HCID 21874036HCID 21874036, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 4N solution of hydrochloric acid in dioxane (122 ml, 488 mmol) was added dropwise to a stirred solution of 5-tert-butyl 1-ethyl 3-{[4-(4-methylpiperazin-1-yl)benzoyl]amino}-4,6-dihydropyrrolo[3,4-c]pyrazole-1,5-dicarboxylate (19.5 g, 39.2 mmol), as prepared in Example 2, in dry DCM (240 ml); precipitation of a white solid occurred almost immediately. The resulting mixture was stirred at room temperature for 24 hours; after dilution with Et20 (100 ml), the solid was filtered, extensively washed with Et20, and dried under vacuum at 50° C. to give 20.1 g of the title compound, used in the next step without further purification. [M+H]+ 399.

후처리

  1. customprecipitation of a white solid
  2. filtrationafter dilution with Et20 (100 ml), the solid was filtered
  3. washextensively washed with Et20
  4. customdried under vacuum at 50° C.

출처 및 근거

ORD 기록
ord-8c53e5bb91ae496688a3b3c521441391
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582628B2

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