Hydrochloric Acid → (E)-3-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-acrylic acid

HRID 403484노트

반응식

HRID 403484 반응식
C[O:2][C:3](=[O:26])/[CH:4]=[CH:5]/[C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13]2[C:14]([CH2:24][CH3:25])=[N:15][N:16]3[C:21]([CH3:22])=[CH:20][C:19]([CH3:23])=[N:18][C:17]=23)=[CH:8][CH:7]=1.[Li+].[OH-].Cl>C1COCC1>[CH2:24]([C:14]1[C:13]([CH2:12][C:9]2[CH:8]=[CH:7][C:6](/[CH:5]=[CH:4]/[C:3]([OH:26])=[O:2])=[CH:11][CH:10]=2)=[C:17]2[N:18]=[C:19]([CH3:23])[CH:20]=[C:21]([CH3:22])[N:16]2[N:15]=1)[CH3:25]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 68379176(E)-3-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-acrylic acid methyl ester

생성물 1

HCID 68378968(E)-3-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-acrylic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

(E)-3-[4-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-acrylic acid methyl ester (4) (2.94 g, 8.4 mmol) was dissolved in 25 ml of THF and 1M LiOH (25 ml) was added. The reaction mixture was stirred over night at rt. Then 0.5M HCl was added until a pH of 3.5 was reached. The mixture was extracted twice with EtOAc, the organic layer was washed with brine and dried over Na2 SO4. After evaporation the product was purified by recrystallisation from EtOAc to give a white solid.

후처리

  1. extractionThe mixture was extracted twice with EtOAc
  2. washthe organic layer was washed with brine
  3. customdried over Na2 SO4
  4. customAfter evaporation the product
  5. customwas purified by recrystallisation from EtOAc
  6. customto give a white solid

출처 및 근거

ORD 기록
ord-c6ca781fa186467abe9483d052a58f0e
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748435B2

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