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Hydrochloric Acid → 5-phenyl-1H-thieno[3,2-c]pyrazole

HRID 2078717
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HRID 2078717 반응식
[C:1]1([C:7]2[S:14][C:13]3[CH:12]=[N:11][N:10](C(=O)C)[C:9]=3[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O)C.Cl.C(=O)([O-])[O-].[K+].[K+]>O>[C:1]1([C:7]2[S:14][C:13]3[CH:12]=[N:11][NH:10][C:9]=3[CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 11430Potassium CarbonateHCID 576373781-(5-Phenyl-thieno[3,2-c]pyrazol-1-yl)-ethanone2회

생성물 1

HCID 576373325-phenyl-1H-thieno[3,2-c]pyrazole수율 92.6%

시약·촉매·용매 1

HCID 962Water
용매

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온도
70 °C

실험 절차

To a mixture of 1-(5-phenyl-thieno[3,2-c]pyrazol-1-yl)-ethanone [3.82 g, 15.8 mmol, Intermediate (44)] and ethanol (50 mL) was added 6 N hydrochloric acid (50.0 mL, 300 mmol) in one portion and the resulting mixture heated at 70° C. After 18 hours, the reaction was cooled to ambient temperature and neutralized with 25% aqueous potassium carbonate. The mixture was diluted with water (200 mL) and aged at 0° C. for 1 hour. The resulting solid was collected, washed three times with water (50 mL), and then dried under vacuum to give 5-phenyl-1H-thieno[3,2-c]pyrazole [2.93 g, 92%, Intermediate (45)] as a beige powder. LC/MS: 201.0 (M+H), RT=3.15 minutes).

후처리

  1. waitaged at 0° C. for 1 hour
  2. customThe resulting solid was collected
  3. washwashed three times with water (50 mL)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-6b1eabc10bbc492da91a9561fe4e5315
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928231B2

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