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

HRID 1357434노트

반응식

HRID 1357434 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b0ab96fe91b645c191b4b56782c7276d
출처 데이터셋
uspto-grants-2003_07
특허 번호
USRE038188E1

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