Ethanol → HCID 178509104, 화합물

HRID 588597노트

반응식

HRID 588597 반응식
[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

참가 물질

6

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 178474487HCID 178474487, 화합물

생성물 1

HCID 178509104HCID 178509104, 화합물수율 49.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5a9f6960b04d4124987d54b8927144ce
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227976B2

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