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Hydrochloric Acid → 5-(7-(Cyclopropylamino)-3-formylpyrazolo[1,5-a]pyrimidin-5-yl)thiophene-2-carboxylic acid

HRID 624751
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인쇄 미리보기

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HRID 624751 반응식
C(OC([N:8]([CH:28]1[CH2:30][CH2:29]1)[C:9]1[N:14]2[N:15]=[CH:16][C:17]([CH:18]=[O:19])=[C:13]2[N:12]=[C:11]([C:20]2[S:24][C:23]([C:25]([OH:27])=[O:26])=[CH:22][CH:21]=2)[CH:10]=1)=O)(C)(C)C.Cl>O1CCOCC1>[CH:28]1([NH:8][C:9]2[N:14]3[N:15]=[CH:16][C:17]([CH:18]=[O:19])=[C:13]3[N:12]=[C:11]([C:20]3[S:24][C:23]([C:25]([OH:27])=[O:26])=[CH:22][CH:21]=3)[CH:10]=2)[CH2:29][CH2:30]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 583139645-(7-(Tert-butoxycarbonyl(cyclopropyl)amino)-3-formylpyrazolo[1,5-a]pyrimidin-5-yl)thiophene-2-carboxylic acid

생성물 1

HCID 583142305-(7-(Cyclopropylamino)-3-formylpyrazolo[1,5-a]pyrimidin-5-yl)thiophene-2-carboxylic acid수율 82%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

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온도
80 °C

실험 절차

To 5-(7-(tert-butoxycarbonyl(cyclopropyl)amino)-3-formylpyrazolo[1,5-a]pyrimidin-5-yl)thiophene-2-carboxylic acid (1 g, 2.33 mmol) was added 8 mL of 4M HCl in dioxane and another 5 mL of dioxane. The reaction mixture was stirred at 80° C. for 2 hours, cooled to room temperature and partitioned between CH2Cl2 and H2O. The emulsion that formed between the layers was filtered off and rinsed with H2O. The recovered solid was dried under vacuum to provide 627 mg of 5-(7-(cyclopropylamino)-3-formylpyrazolo[1,5-a]pyrimidin-5-yl)thiophene-2-carboxylic acid as a red solid (82%). LCMS (M+1=329)

후처리

  1. temperaturecooled to room temperature
  2. custompartitioned between CH2Cl2 and H2O
  3. customThe emulsion that formed between the layers
  4. filtrationwas filtered off
  5. washrinsed with H2O
  6. customThe recovered solid was dried under vacuum

출처 및 근거

ORD 기록
ord-fd0c48a108ee4ab2b3fcdfb02689919b
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09303033B2

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