2-Mercapto-2-methylpropanoic acid → 2-{[2-(3,5-Difluorophenyl)-2-oxoethyl]thio}-2-methylpropanoic acid

HRID 1866608

反応式

HRID 1866608 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5](=[O:8])[CH2:6]Br.C(=O)(O)[O-].[Na+].[SH:18][C:19]([CH3:24])([CH3:23])[C:20]([OH:22])=[O:21]>C1COCC1.O.C(OCC)C.Cl>[F:1][C:2]1[CH:3]=[C:4]([C:5](=[O:8])[CH2:6][S:18][C:19]([CH3:24])([CH3:23])[C:20]([OH:22])=[O:21])[CH:9]=[C:10]([F:12])[CH:11]=1

参加物

8

反応物 3

HCID 784212-Mercapto-2-methylpropanoic acidHCID 516892Sodium BicarbonateHCID 27783312-Bromo-1-(3,5-difluorophenyl)ethanone

生成物 1

HCID 669733052-{[2-(3,5-Difluorophenyl)-2-oxoethyl]thio}-2-methylpropanoic acid

試薬・触媒・溶媒 4

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3,5-difluorophenacyl bromide (845 mg, 3.60 mmol) in THF (12 mL) and water (12 mL) was added sodium bicarbonate (317 mg, 3.78 mmol) and 2-mercaptoisobutyric acid (432 mg, 3.60 mmol). The reaction mixture was allowed to stir at ambient temperature for 1.0 h under a stream of nitrogen. The reaction mixture was diluted with diethyl ether (50 mL) and 1 M HCl (15 mL). The organic layer was then washed with 20 mL saturated brine. The organics were then dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound, which was used without further purification. MS: m/z=229 (M−CO2H).

後処理

  1. washThe organic layer was then washed with 20 mL saturated brine
  2. dry with materialThe organics were then dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-49e89eca02ac408497475da47ed5bce4
出典データセット
uspto-grants-2009_12
特許番号
US07629338B2

関連ノート

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