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

HRID 2036969
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HRID 2036969 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-8cfaedfb2a024bdbb82b20e4b2fccfdf
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08575177B2

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