Potassium Carbonate → HCID 71087246、化合物

HRID 571882ノート

反応式

HRID 571882 の反応式
[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

参加物

5

反応物 2

HCID 11430Potassium Carbonate2 回HCID 71086736HCID 71086736、化合物

生成物 1

HCID 71087246HCID 71087246、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e48d97ec530440688a6e5735f50ca842
出典データセット
uspto-grants-2015_05
特許番号
US09029370B2

反応ノート

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