Hydrochloric Acid → 2-(4-Methoxy-3-((4-(trifluoromethyl)benzamido)methyl)benzyl)butanoic acid

HRID 1826087ノート

反応式

HRID 1826087 の反応式
[CH2:1]([CH:3]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH2:18][NH:19][C:20](=[O:31])[C:21]2[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=2)[CH:11]=1)[C:4]([O:6]CC)=[O:5])[CH3:2].CO.[OH-].[Na+].Cl>O>[CH2:1]([CH:3]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH2:18][NH:19][C:20](=[O:31])[C:21]2[CH:22]=[CH:23][C:24]([C:27]([F:29])([F:28])[F:30])=[CH:25][CH:26]=2)[CH:11]=1)[C:4]([OH:6])=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 11004633Ethyl 2-[4-methoxy-3-({[4-(trifluoromethyl)benzoyl]amino}methyl)benzyl]butanoate

生成物 1

HCID 102015452-(4-Methoxy-3-((4-(trifluoromethyl)benzamido)methyl)benzyl)butanoic acid収率 99%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

A mixture of ethyl 2-ethyl-3-[3-[4-(trifluoromethyl)benzoylaminomethyl]-4-methoxyphenyl]propanoate (240 mg, 0.549 mmol), methanol (6 mL) and 2.5 mol/L aqueous solution of sodium hydroxide (2 mL) was stirred for 4 hours under heating at 50° C. After cooling, water (20 mL) was added and the mixture was made acidic with 1 mol/L hydrochloric acid, which was then extracted with ethyl acetate. The organic later was washed with water and brine, dried over anhydrous sodium sulfate, and then concentrated to afford 222 mg (99%) of the title compound as colorless crystals. Further, these were recrystallized from diethyl ether-n-hexane, thus affording 161 mg (72%) of purified title compound as colorless needles.

後処理

  1. temperatureAfter cooling
  2. extractionwas then extracted with ethyl acetate
  3. washThe organic later was washed with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8b3b781c090443d4b29c4da573960419
出典データセット
uspto-grants-2006_05
特許番号
US07049342B2

反応ノート

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