Sodium Hydroxide → 2-(2,5-Dichloro-4-methoxyphenyl)acetic acid

HRID 1930122

反応式

HRID 1930122 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([Cl:10])=[CH:4][C:3]=1[CH:11](C(OCC)=O)[C:12]([O:14]CC)=[O:13].[OH-].[Na+]>C1COCC1.CCO>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([Cl:10])=[CH:4][C:3]=1[CH2:11][C:12]([OH:14])=[O:13]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 59627728Diethyl 2-(2,5-dichloro-4-methoxyphenyl)malonate2 回

生成物 1

HCID 52022252-(2,5-Dichloro-4-methoxyphenyl)acetic acid収率 60.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A solution of diethyl 2-(2,5-dichloro-4-methoxyphenyl)malonate (Intermediate 4-5; 1.88 g, 5.61 mmol) in THF (55 mL) and EtOH (5 mL) was treated with 2M sodium hydroxide (11.22 mL, 22.44 mmol) in one portion and the resulting solution was stirred at 60° C. for 17 hours. The reaction mixture was evaporated and the aqueous residue was acidified with 2M HCl. The precipitate was collected by filtration, washed with water (25 mL) and dried under vacuum to afford 2-(2,5-dichloro-4-methoxyphenyl)acetic acid (0.800 g, 60.7%) as a grey solid, which was used without further purification.

後処理

  1. customThe reaction mixture was evaporated
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water (25 mL)
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-1c6b304e486b48c9804a207ee40507f9
出典データセット
uspto-grants-2012_05
特許番号
US08188092B2

関連ノート

読み込み中…