Water → 2-(2-Cyclobutoxy-3-methyl-benzoylamino)-5-fluoro-indan-2-carboxylic acid

HRID 1047754노트

반응식

HRID 1047754 반응식
C([O:3][C:4]([C:6]1([NH:16][C:17](=[O:30])[C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:19]=2[O:25][CH:26]2[CH2:29][CH2:28][CH2:27]2)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([F:15])[CH:12]=2)[CH2:7]1)=[O:5])C.[OH-].[K+].O>CCO>[CH:26]1([O:25][C:19]2[C:20]([CH3:24])=[CH:21][CH:22]=[CH:23][C:18]=2[C:17]([NH:16][C:6]2([C:4]([OH:5])=[O:3])[CH2:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([F:15])[CH:12]=3)[CH2:7]2)=[O:30])[CH2:27][CH2:28][CH2:29]1

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 593142022-(2-Cyclobutoxy-3-methyl-benzoylamino)-5-fluoro-indan-2-carboxylic acid ethyl ester

생성물 1

HCID 251606672-(2-Cyclobutoxy-3-methyl-benzoylamino)-5-fluoro-indan-2-carboxylic acid수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The mixture of 2-(2-cyclobutoxy-3-methyl-benzoylamino)-5-fluoro-indan-2-carboxylic acid ethyl ester (102) (510 mg, 1.24 mmol) and KOH (1 g, 18 mmol) is dissolved in EtOH (8 mL) and water (1 mL) under a water bath. The water bath is removed when KOH is completely dissolved and the resulting reaction solution is stirred at RT for 8 h. After concentration in vacuo, the residue is dissolved in water (20 mL) and acidified with conc. HCl until no more white precipitate formed. The precipitate is filtered to give a pure product (103) as white solid (469 mg, 99%).

후처리

  1. customThe water bath is removed when KOH
  2. dissolutionis completely dissolved
  3. customthe resulting reaction solution
  4. concentrationAfter concentration in vacuo
  5. dissolutionthe residue is dissolved in water (20 mL)
  6. customformed
  7. filtrationThe precipitate is filtered

출처 및 근거

ORD 기록
ord-291dc40f283548408b13481eab5f5831
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569535B2

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