Potassium Carbonate → HCID 71087246, 화합물

HRID 571882노트

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HRID 571882 반응식
[F:1][C:2]([F:20])([F:19])[C:3]1[N:8]=[C:7]([N:9]2[CH:13]=[C:12]([C:14]([O:16]CC)=[O:15])[CH:11]=[N:10]2)[CH:6]=[N:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[F:20][C:2]([F:1])([F:19])[C:3]1[N:8]=[C:7]([N:9]2[CH:13]=[C:12]([C:14]([OH:16])=[O:15])[CH:11]=[N:10]2)[CH:6]=[N:5][CH:4]=1

참가 물질

5

반응물 2

HCID 11430Potassium Carbonate2회HCID 71086736HCID 71086736, 화합물

생성물 1

HCID 71087246HCID 71087246, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

Under N2, ethyl 1-(6-(trifluoromethyl)pyrazin-2-yl)-1H-pyrazole-4-carboxylate (155 mg, 542 μmol, Eq: 1.00) was dissolved in DMF (9.3 ml) and Water (9.3 ml). Potassium carbonate (150 mg, 1.08 mmol, Eq: 2) was added and the RM was stirred at 70° C. overnight. Control with LC-MS: Pr/SM: 74/26. Potassium carbonate (150 mg, 1.08 mmol, Eq: 2) was added and the RM was stirred at 70° C. overnight. Control with LC-MS: SM/Pr:4/96. At RT, the RM was partitioned between 1M K2CO3 and EtOAc; extracted; the water layer was acidified with 1M HCl; extracted with EtOAc; the organic phase was dried over MgSO4; filtered; concentrated in vacuo leading to 132 mg off-white solid.

후처리

  1. stirringthe RM was stirred at 70° C. overnight
  2. customAt RT, the RM was partitioned between 1M K2CO3 and EtOAc
  3. extractionextracted
  4. extractionextracted with EtOAc
  5. dry with materialthe organic phase was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e48d97ec530440688a6e5735f50ca842
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029370B2

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