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Sodium Hydroxide → HCID 59631853, 화합물

HRID 2369040
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HRID 2369040 반응식
C[O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]2[S:11][C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([S:21]([CH3:24])(=[O:23])=[O:22])[CH:16]=3)=[CH:13][CH:14]=2)[N:7]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[Cl:31])[N:6]=1)=[O:4].[OH-].[Na+]>CO>[Cl:31][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[N:7]1[C:8]([C:10]2[S:11][C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([S:21]([CH3:24])(=[O:22])=[O:23])[CH:16]=3)=[CH:13][CH:14]=2)=[CH:9][C:5]([C:3]([OH:4])=[O:2])=[N:6]1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 59631939HCID 59631939, 화합물

생성물 1

HCID 59631853HCID 59631853, 화합물수율 9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

To a solution of 1-(2-chloro-phenyl)-5-[5-(3-methanesulfonyl-phenyl)-thiophen-2-yl]-1H-pyrazole-3-carboxylic acid methyl ester (5.8 g, 123 mmol) in MeOH (50 mL) was added aqueous NaOH (4 N, 25 mL) and the mixture was refluxed for 2 h. After cooling to 20° C., solvent was removed. Water was added to dissolve the crude and then the solution was acidified with acetic acid. Solid was collected by filtration and washed with water and dried under high vacuum to give 1-(2-chlorophenyl)-5-{5-[3-(methylsulfonyl)phenyl]-2-thienyl}-1H-pyrazole-3-carboxylic acid (5.1 g). MS(ES): 459 [M+H]+.

후처리

  1. temperaturethe mixture was refluxed for 2 h
  2. customsolvent was removed
  3. additionWater was added
  4. dissolutionto dissolve the crude
  5. filtrationSolid was collected by filtration
  6. washwashed with water
  7. customdried under high vacuum

출처 및 근거

ORD 기록
ord-d54decbe437c49c1ba02bf52a65eab83
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703805B2

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