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Hydrochloric Acid → 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamide

HRID 2364073
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HRID 2364073 반응식
CC1(C)[NH:7][C:6]2[CH:8]=[C:9]([C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH3:16])[S:10][C:5]=2[C:4](=[O:17])[NH:3]1.Cl>CO>[NH2:7][C:6]1[CH:8]=[C:9]([C:11]2[CH:12]=[N:13][NH:14][C:15]=2[CH3:16])[S:10][C:5]=1[C:4]([NH2:3])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66743505Cdc7-IN-15

생성물 1

HCID 667430133-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamide수율 72%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 2,2-dimethyl-6-(5-methyl-1H-pyrazol-4-yl)-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one (1.97 g, 7.51 mmol), 1 M aqueous HCl. (38 mL) and MeOH (38 mL) was stirred at 50° C. for 4 h. After removal of the solvent at reduced pressure, the organic materials were extracted with EtOAc/THF. The combined extracts were dried over Na2SO4 and filtered. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH) to give the title compound (1.20 g, 72%) as a green solid:

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후처리

  1. customAfter removal of the solvent at reduced pressure
  2. extractionthe organic materials were extracted with EtOAc/THF
  3. dry with materialThe combined extracts were dried over Na2SO4
  4. filtrationfiltered
  5. customAfter removal of the solvent at reduced pressure
  6. customthe residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH)

출처 및 근거

ORD 기록
ord-d365f5cec34a4d97ab8567ace77df18c
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691828B2

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