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Water → 5-Chloro-2-(4-fluorophenyl)-2-methoxyvaleric acid

HRID 1009401
ノート
印刷プレビュー

反応式

HRID 1009401 の反応式
[OH-].[Na+].[Cl:3][CH2:4][CH2:5][CH2:6][C:7]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)([O:12][CH3:13])[C:8]([O:10]C)=[O:9].O>C1COCC1.CO>[Cl:3][CH2:4][CH2:5][CH2:6][C:7]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)([O:12][CH3:13])[C:8]([OH:10])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 14798Sodium Hydroxide2 回HCID 67067459Methyl 5-chloro-2-(4-fluorophenyl)-2-methoxyvalerate

生成物 1

HCID 670671515-Chloro-2-(4-fluorophenyl)-2-methoxyvaleric acid収率 81.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒

実験手順

A 4 N sodium hydroxide solution (0.2 mL) was added to a mixed solution of methyl 5-chloro-2-(4-fluorophenyl)-2-methoxyvalerate (141 mg) in THF (1 mL) and methanol (0.5 mL), and the reaction solution was stirred at room temperature for 3.5 hours. Methanol (0.5 mL) and a 4 N sodium hydroxide solution (0.1 mL) were added to the reaction solution, and the reaction solution was further stirred at room temperature for 1.5 hours. Water was added to the reaction solution which was then washed with diethyl ether. 1 N hydrochloric acid (1.4 mL) and ethyl acetate were added to the resulting aqueous layer, and the organic layer was separated. The resulting ethyl acetate layer was washed with brine and dried over anhydrous magnesium sulfate. The resulting ethyl acetate layer was concentrated under reduced pressure to obtain 109 mg of the title compound. The property values of the compound are as follows.

後処理

  1. stirringthe reaction solution was further stirred at room temperature for 1.5 hours
  2. washwas then washed with diethyl ether
  3. addition1 N hydrochloric acid (1.4 mL) and ethyl acetate were added to the resulting aqueous layer
  4. customthe organic layer was separated
  5. washThe resulting ethyl acetate layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe resulting ethyl acetate layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-7737f7c569a744fa9154a4b1e1447cc4
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07973033B2

反応ノート

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