Ethanol → HCID 178509104、化合物

HRID 1615715ノート

反応式

HRID 1615715 の反応式
[C:1]1([C:7]2[C:11]([C:12]#[C:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[C:10]([NH:20]C(=O)C)[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O)C.[OH-].[Na+]>C(OCC)(=O)C.O>[C:1]1([C:7]2[C:11]([C:12]#[C:13][C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)=[C:10]([NH2:20])[NH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 178474487HCID 178474487、化合物

生成物 1

HCID 178509104HCID 178509104、化合物収率 49.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

A mixture of N-[3-phenyl-4-(2-phenylethynyl)-1H-pyrazol-5-yl]acetamide (12.5 g, 42 mmol), ethanol (100 mL) and 25% aq. NaOH solution (100 mL) was stirred and heated to 90° C. for 1 h and cooled to room temperature. The reaction mixture was diluted with ethyl acetate and water. The organic phase was washed with water and brine, dried (phase separator cartridge) and concentrated in vacuo. Diethyl ether was added to the residue and the solid was collected by filtration, washed with diethyl ether and dried in vacuo to provide the title compound as a solid (5.4 g).

後処理

  1. temperaturecooled to room temperature
  2. washThe organic phase was washed with water and brine
  3. customdried (phase separator cartridge)
  4. concentrationconcentrated in vacuo
  5. additionDiethyl ether was added to the residue
  6. filtrationthe solid was collected by filtration
  7. washwashed with diethyl ether
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-b0062d4a807c4b718997a7ca8d6c7e0e
出典データセット
uspto-grants-2014_07
特許番号
US08765762B2

反応ノート

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