Water → Ethyl 2-phenyl-3-(3,5-dichloro-1-methylpyrazol-4-yl)-3-hydroxyacrylate

HRID 1107691ノート

反応式

HRID 1107691 の反応式
[C:1]1([CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:13][C:14]1[C:18]([C:19](Cl)=[O:20])=[C:17]([Cl:22])[N:16]([CH3:23])[N:15]=1.CC(C)([O-])C.[K+].O>O1CCCC1>[C:1]1([C:7](=[C:19]([C:18]2[C:14]([Cl:13])=[N:15][N:16]([CH3:23])[C:17]=2[Cl:22])[OH:20])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 962WaterHCID 7590Ethyl phenylacetateHCID 221694993,5-Dichloro-1-methylpyrazole-4-carbonyl chlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 57189495Ethyl 2-phenyl-3-(3,5-dichloro-1-methylpyrazol-4-yl)-3-hydroxyacrylate収率 99.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

8.2 g (50 mmols) of ethyl phenylacetate and 10.7 g (50 mmols) of 3,5-dichloro-1-methylpyrazole-4-carboxylic acid chloride were dissolved in 100 ml of dry tetrahydrofuran, and 14 g (125 mmols) of potassium tert-butoxide at room temperature. The reaction mixture was stirred at room temperature for 1 hour, and 300 ml of water was added thereto, and extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 17 g of the intended ethyl 2-phenyl-3-(3,5-dichloro-1-methylpyrazol-4-yl)-3-hydroxyacrylate.

後処理

  1. customat room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-d4e5ea9c93d24a21861ca4726ab84cf0
出典データセット
uspto-grants-2000_05
特許番号
US06063734

反応ノート

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