Acetic Acid → HCID 57411216, 화합물

HRID 623907노트

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HRID 623907 반응식
[CH:1]1([CH2:4][C:5]2[NH:9][C:8]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[C:17]([CH3:31])=[CH:18][C:19]([O:22][CH2:23][C:24]([CH3:30])([CH3:29])[C:25]([O:27]C)=[O:26])=[N:20][CH:21]=4)=[CH:12][C:11]=3[F:32])=[N:7][CH:6]=2)[CH2:3][CH2:2]1.[OH-].[Na+].O.C(O)(=O)C>O1CCCC1.CO>[CH:1]1([CH2:4][C:5]2[NH:9][C:8]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[C:17]([CH3:31])=[CH:18][C:19]([O:22][CH2:23][C:24]([CH3:29])([CH3:30])[C:25]([OH:27])=[O:26])=[N:20][CH:21]=4)=[CH:12][C:11]=3[F:32])=[N:7][CH:6]=2)[CH2:2][CH2:3]1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 67975334HCID 67975334, 화합물

생성물 1

HCID 57411216HCID 57411216, 화합물수율 141.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

In tetrahydrofuran (10 mL) and methanol (10 mL) was dissolved methyl 3-[(5-{4-[5-(cyclopropylmethyl)-1H-imidazol-2-yl]-3-fluorophenyl}-4-methylpyridin-2-yl)oxy]-2,2-dimethylpropanoate (247 mg), and after adding 2N aqueous sodium hydroxide solution (2.8 mL) to the solution, the resulting mixture was stirred at 50° C. for 7 hours. Water and acetic acid were added to the residue obtained by concentrating the reaction mixture under reduced pressure. The precipitated solid was collected by filtration, washed with water and dried to obtain 3-[(5-{4-[5-(cyclopropylmethyl)-1H-imidazol-2-yl]-3-fluorophenyl}-4-methylpyridin-2-yl)oxy]-2,2-dimethylpropanoic acid (339 mg).

후처리

  1. customobtained
  2. concentrationby concentrating the reaction mixture under reduced pressure
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-eb8ec26f993e4127b0a2fc34aec63d95
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302996B2

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