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Dichloromethane → Chloromethyl 2-(4-(4-chlorobenzoyl)phenoxy)-2-methylpropanoate

HRID 571347
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HRID 571347 반응식
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]([C:6]([C:8]2[CH:20]=[CH:19][C:11]([O:12][C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)(O)[O-].[Na+].[Cl:28][CH2:29]Cl.CCCCCC>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[Cl:1][C:2]1[CH:22]=[CH:21][C:5]([C:6]([C:8]2[CH:20]=[CH:19][C:11]([O:12][C:13]([CH3:18])([CH3:17])[C:14]([O:16][CH2:29][Cl:28])=[O:15])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 8058HexaneHCID 64929Fenofibric AcidHCID 516892Sodium Bicarbonate

생성물 1

HCID 57586167Chloromethyl 2-(4-(4-chlorobenzoyl)phenoxy)-2-methylpropanoate수율 101%

시약·촉매·용매 2

HCID 94433
Tetrabutylammonium hydrogen sulfate
촉매
HCID 962Water용매

실험 절차

A mixture of 2-(4-(4-chlorobenzoyl)phenoxy)-2-methylpropanoic acid (10.0 g, 31.4 mmol), sodium bicarbonate (13.2 g, 47.1 mmol, 1.5 eq) and tetrabutylammonium hydrogensulfate (2.1 g, 6.3 mmol, 0.2 eq) in water (150 mL) was stirred at room temperature for 15 min. Dichloromethane (150 mL) was added and the mixture was cooled in ice. Chloromethyl sulfochloridate (4.2 mL, 47.1 mmol, 1.5 eq) was added and the mixture was stirred overnight at room temperature. The layers were separated, the organic phase was washed with water (50 mL) and brine, then dried over sodium sulfate. The drying agent was filtered off and the solution was concentrated by rotary evaporation to leave a thick oil. Hexane (50 mL) and seeds were added and rotary evaporation was continued at room temperature to leave chloromethyl 2-(4-(4-chlorobenzoyl)phenoxy)-2-methylpropanoate 1 as a white solid (11.6 g, 101% yield). 1H-NMR (CDCl3) δ 7.73 (d, 2 H), 7.70 (d, 2 H), 7.44 (d, 2 H), 6.87 (d, 2 H), 5.77, (s, 2 H), 1.70 (s, 6 H) ppm.

후처리

  1. temperaturethe mixture was cooled in ice
  2. additionChloromethyl sulfochloridate (4.2 mL, 47.1 mmol, 1.5 eq) was added
  3. stirringthe mixture was stirred overnight at room temperature
  4. customThe layers were separated
  5. washthe organic phase was washed with water (50 mL) and brine
  6. dry with materialdried over sodium sulfate
  7. filtrationThe drying agent was filtered off
  8. concentrationthe solution was concentrated by rotary evaporation
  9. customto leave a thick oil
  10. customrotary evaporation
  11. customwas continued at room temperature

출처 및 근거

ORD 기록
ord-37e1aed844594d4e9253087802b89949
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09024069B2

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