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Sodium Hydroxide → HCID 70664978, 화합물

HRID 1854529
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HRID 1854529 반응식
[H-].[Na+].[NH2:3][C:4]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2F)[N:7]=[C:6]([C:16]([O:18]CC)=[O:17])[CH:5]=1.[OH-:21].[Na+]>O1CCOCC1>[C:9]1([N:8]2[C:4]([NH:3][C:4]([NH:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)=[O:21])=[CH:5][C:6]([C:16]([OH:18])=[O:17])=[N:7]2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 53302142Ethyl 5-amino-1-(2-fluorophenyl)-1H-pyrazole-3-carboxylate

생성물 1

HCID 70664978HCID 70664978, 화합물수율 26%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

145.3 mg (3.63 mmol, 1.2 Eq) of a 60% suspension of NaH in mineral oil are suspended in 25 ml of dioxane, 700 mg (3.03 mmol) of ethyl 5-amino-1-(2-fluoro-phenyl)-1H-pyrazole-3-carboxylate are added and the resulting mixture is stirred for 10 minutes at RT: Then phenylisocanate (360.6 mg, 3.03 mmol, 1 Eq) is added and the resulting mixture is heated to 80° C. for 5 hours. After cooling 7 ml of 1M NaOH are added and the resulting mixture is stirred overnight at RT. The solvent is evaporated in vacuo and the obtained crude product is subjected to HPLC chromatography. 257 mg (26%) of the pure product are obtained.

후처리

  1. additionphenylisocanate (360.6 mg, 3.03 mmol, 1 Eq) is added
  2. temperaturethe resulting mixture is heated to 80° C. for 5 hours
  3. additionare added
  4. stirringthe resulting mixture is stirred overnight at RT
  5. customThe solvent is evaporated in vacuo
  6. customthe obtained crude product

출처 및 근거

ORD 기록
ord-27625576d38e4611861358c77365e4e1
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08962671B2

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