Hydrochloric Acid → HCID 57742536、化合物

HRID 2266491ノート

反応式

HRID 2266491 の反応式
C[O:2][C:3](=[O:30])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([CH3:29])=[C:9]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=1)[C:10]([O:17][CH:18]([F:20])[F:19])=[N:11]2.O1CCCC1.[OH-].[Li+].Cl>CO>[Cl:28][C:25]1[CH:24]=[CH:23][C:22]([CH2:21][C:9]2[C:10]([O:17][CH:18]([F:19])[F:20])=[N:11][C:12]3[C:7]([C:8]=2[CH3:29])=[C:6]([O:5][CH2:4][C:3]([OH:30])=[O:2])[CH:15]=[CH:14][C:13]=3[F:16])=[CH:27][CH:26]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 68785003HCID 68785003、化合物

生成物 1

HCID 57742536HCID 57742536、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of [3-(4-chlorobenzyl)-2-difluoromethoxy-8-fluoro-4-methylquinolin-5-yloxy]acetic acid methyl ester (0.45 g), tetrahydrofuran (5.0 mL), methanol (5.0 mL) and 1.0 M aqueous lithium hydroxide solution (1.3 mL) was stirred at room temperature for 18 hours. The solution was acidified by the addition of 1.0 M aqueous hydrochloric acid and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. Crystallisation of the residue from a mixture of water and propan-2-ol gave title compound as a white solid, 0.33 g.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined extracts were dried over magnesium sulfate
  3. customthe solvent removed under reduced pressure
  4. customCrystallisation of the residue
  5. additionfrom a mixture of water and propan-2-ol

出典と根拠

ORDレコード
ord-f5cbb573ff4b4a3d8bf523c5985d8d11
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

反応ノート

読み込み中…