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Sulfuryl chloride → Methyl 2-chloro-3-oxoheptanoate

HRID 2103428
ノート
印刷プレビュー

反応式

HRID 2103428 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 546075Methyl 3-oxoheptanoate

生成物 1

HCID 57713025Methyl 2-chloro-3-oxoheptanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2565377f9e8e454297a4b8200e94c088
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576109B2

反応ノート

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