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

HRID 34510

반응식

HRID 34510 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 91760Sulcotrione

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-(2-Chloro-4-methanesulfonylbenzoyl)-cyclohexane-1,3-dione (9.8 g, 30 millimole) was dissolved in 100 ml methylene chloride and stirred at room temperature. To this solution was added oxalyl chloride (5.7 g, 45 mmol) 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 and then dried with MgSO4 and the solvent evaporated to yield 3-chloro-2-(2chloro-4-methanesulfonylbenzoyl)cyclohex-2-enone (7.3 g, 70%) as an oil which was used without further purification.

후처리

  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 materialdried with MgSO4
  5. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-34728028b01f47d2ac4cf2ff27836909
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762551

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