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Acetic Acid → Niraxostat

HRID 850071
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HRID 850071 반응식
[C:1]([C:3]1[CH:4]=[C:5]([N:15]2[CH:19]=[C:18]([C:20]([O:22]CC)=[O:21])[CH:17]=[N:16]2)[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])#[N:2].[OH-].[Na+].O.C(O)(=O)C>C(O)C>[C:1]([C:3]1[CH:4]=[C:5]([N:15]2[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[N:16]2)[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])#[N:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 19366044HCID 19366044, 화합물

생성물 1

HCID 449035Niraxostat수율 38.3%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To a solution (20 ml) of ethyl 1-(3-cyano-4-neopentyloxyphenyl)pyrazole4-carboxylate (2 g) in ethanol was added 2 N aqueous sodium hydroxide solution (3.7 ml) with stirring, and the mixture was heated at 80° C. for 30 minutes. After the completion of the reaction, the reaction mixture was poured into water and neutralized with acetic acid. The precipitated crystals were recrystallized from a mixed solution of ethyl alcohol and water to give 0.7 g of 1-(3-cyano-4-neopentyloxyphenyl) pyrazole-4-carboxylic acid, melting point 199-200° C.

후처리

  1. customAfter the completion of the reaction
  2. customThe precipitated crystals were recrystallized from a mixed solution of ethyl alcohol and water

출처 및 근거

ORD 기록
ord-93cb202be4284160b65e90aa7dbb5fb1
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06015829

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