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Dimethyl Sulfone → 1-[3,5-Bis(dimethylamino)-4-methylphenyl]-2-(methanesulfonyl)ethan-1-one

HRID 1413731
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HRID 1413731 반응식
[CH3:1][S:2]([CH3:5])(=[O:4])=[O:3].[H-].[Na+].[CH3:8][N:9]([CH3:24])[C:10]1[CH:11]=[C:12]([CH:17]=[C:18]([N:21]([CH3:23])[CH3:22])[C:19]=1[CH3:20])[C:13](OC)=[O:14]>CS(C)=O>[CH3:23][N:21]([CH3:22])[C:18]1[CH:17]=[C:12]([C:13](=[O:14])[CH2:1][S:2]([CH3:5])(=[O:4])=[O:3])[CH:11]=[C:10]([N:9]([CH3:24])[CH3:8])[C:19]=1[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6213Dimethyl SulfoneHCID 24758Sodium hydrideHCID 20290395Methyl 3,5-bis(dimethylamino)-4-methylbenzoate

생성물 1

HCID 202903891-[3,5-Bis(dimethylamino)-4-methylphenyl]-2-(methanesulfonyl)ethan-1-one

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A suspension of 18.8 g. of dimethylsulfone and 3.6 g. of sodium hydride (50% dispersion in oil) in 80 ml. of dimethylsulfoxide was stirred with the exclusion of moisture for 2 hours at 50° C. Thereupon, 23.6 g. of methyl 3,5-bis(dimethylamino)-4-methylbenzoate were added and the mixture was stirred at room temperature for 1.5 hours. The solution was diluted with 400 ml. of water and extracted twice with ethyl acetate. The ethyl acetate phases were combined, washed with water, dried over sodium sulfate and evaporated to dryness in vacuo. After recrystallization of the residue from methanol, there was obtained 3',5'-bis(dimethylamino)-4'-methyl-2-methylsulfonylacetophenone, having a melting point of 161°-163° C.

후처리

  1. additionA suspension of 18.8 g
  2. additionThe solution was diluted with 400 ml
  3. extractionof water and extracted twice with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated to dryness in vacuo
  7. customAfter recrystallization of the residue from methanol

출처 및 근거

ORD 기록
ord-bd3bc4d32a3f47fcabd79f3ded6a527e
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04251454

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