Water → 3-Chloro-2-[2-chloro-4-(methanesulfonyl)benzoyl]cyclohex-2-en-1-one

HRID 867390

反応式

HRID 867390 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([S:18]([CH3:21])(=[O:20])=[O:19])[CH:15]=[CH:14][C:3]=1[C:4]([CH:6]1[C:11](=[O:12])[CH2:10][CH2:9][CH2:8][C:7]1=O)=[O:5].C(Cl)(=O)C([Cl:25])=O.CN(C)C=O.O>C(Cl)Cl>[Cl:25][C:7]1[CH2:8][CH2:9][CH2:10][C:11](=[O:12])[C:6]=1[C:4](=[O:5])[C:3]1[CH:14]=[CH:15][C:16]([S:18]([CH3:21])(=[O:20])=[O:19])=[CH:17][C:2]=1[Cl:1]

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 91760Sulcotrione

生成物 1

HCID 142799823-Chloro-2-[2-chloro-4-(methanesulfonyl)benzoyl]cyclohex-2-en-1-one収率 70.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(2-Chloro-4-methanesulfonylbenzoyl)-cyclohexane-1,3-dione [9.8 g, 30 millimole (mmol)] was dissolved in 100 ml methylene chloride and stirred at room temperature. To this solution was added oxalyl chloride (5.7 g, 45mmol) followed by dimethylformamide (0.5 ml) in portions small enough to control effervescence. The resulting solution was stirred for 4 hours and then poured into water and extracted with methylene chloride. The organic layer was washed again with water, saturated K2CO3 solution andthen dried with MgSO4 and the solvent evaporated to yield 3-chloro-2(2-chloro-4-methanesulfonylbenzoyl)cyclohex-2-enone (7.3 g, 70%)as an oil which was used without further purification.

後処理

  1. stirringThe resulting solution was stirred for 4 hours
  2. extractionextracted with methylene chloride
  3. washThe organic layer was washed again with water, saturated K2CO3 solution
  4. dry with materialandthen dried with MgSO4
  5. customthe solvent evaporated

出典と根拠

ORDレコード
ord-71c1f3a15f6a404485c9b9fa6f1f9026
出典データセット
uspto-grants-1988_10
特許番号
US04775411

関連ノート

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