Acetic Acid → HCID 57411216、化合物

HRID 623907ノート

反応式

HRID 623907 の反応式
[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

参加物

7

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 67975334HCID 67975334、化合物

生成物 1

HCID 57411216HCID 57411216、化合物収率 141.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eb8ec26f993e4127b0a2fc34aec63d95
出典データセット
uspto-grants-2016_04
特許番号
US09302996B2

反応ノート

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