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Sulfuryl chloride → Methyl 2-chloro-3-oxoheptanoate

HRID 2103428
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HRID 2103428 반응식
[CH3:1][O:2][C:3](=[O:11])[CH2:4][C:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9].S(Cl)([Cl:15])(=O)=O>ClCCl>[CH3:1][O:2][C:3](=[O:11])[CH:4]([Cl:15])[C:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9]
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참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 546075Methyl 3-oxoheptanoate

생성물 1

HCID 57713025Methyl 2-chloro-3-oxoheptanoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-oxo-heptanoic acid methyl ester (5.0 g, 31.6 mmol) in dry dichloromethane (80 mL) add sulfurylchloride (2.82 mL). Stir the reaction mixture at room temperature for 30 minutes then add water (20 mL) and the reaction mixture extracted five times with portions of 30 mL of dichloromethane. Wash the combined organic extracts with water, saturated aqueous solution of NaHCO3 and brine and then dry over MgSO4. Remove the solvent under reduced pressure to give 2-chloro-3-oxo-heptanoic acid methyl ester (6.0 g), which was used in the next step without further purification. To a solution of 2-chloro-3-oxo-heptanoic acid methyl ester (6.0 g, 31.1 mmol) in ethanol (50 mL) add 4-(trifluoromethyl) thiobenzamide (6.4 g, 31.2 mmol). Heat the reaction mixture to reflux overnight. Remove the solvent under reduced pressure and purify the residue by chromatography on silica gel (eluting with a gradient of n-heptane:ethyl acetate (100:1 to 60:1)) to give 4-butyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-carboxylic acid methyl ester (7.4 g) as a yellow oil.

후처리

  1. extractionadd water (20 mL) and the reaction mixture extracted five times with portions of 30 mL of dichloromethane
  2. washWash the combined organic extracts with water, saturated aqueous solution of NaHCO3 and brine
  3. dry with materialdry over MgSO4
  4. customRemove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-2565377f9e8e454297a4b8200e94c088
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576109B2

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