Hydrochloric Acid → 3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetic acid

HRID 1084847노트

반응식

HRID 1084847 반응식
[OH-].[Na+].C(O)C.[F:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[N:15]([C:22]3[CH:23]=[C:24]([CH:32]=[CH:33][CH:34]=3)[O:25][CH2:26][C:27]([O:29]CC)=[O:28])[N:14]=2)=[CH:9][CH:8]=1.Cl>O.O1CCOCC1>[F:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[N:15]([C:22]3[CH:23]=[C:24]([CH:32]=[CH:33][CH:34]=3)[O:25][CH2:26][C:27]([OH:29])=[O:28])[N:14]=2)=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 14796397ethyl 3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetate

생성물 1

HCID 147963983-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetic acid수율 64.6%

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매

실험 절차

In 5 ml of water was dissolved 0.97 g of sodium hydroxide, whereto 100 ml of ethanol was added. Thereto was added a solution of 8.0 g of ethyl 3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetate dissolved in 60 ml of dioxane while stirring. After the mixture was stirred at room temperature for 4 hours, about 500 ml of water was added thereto and the mixture was neutralized with dilute hydrochloric acid. The resulting crystals were collected by filtration and recrystallized from dioxane to give 4.8 g of 3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetic acid, m.p. 225°-226° C.

후처리

  1. additionwas added
  2. stirringAfter the mixture was stirred at room temperature for 4 hours
  3. filtrationThe resulting crystals were collected by filtration
  4. customrecrystallized from dioxane

출처 및 근거

ORD 기록
ord-075ca88072b54f258602ec2a0720b8f2
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05006520

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