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1,1,2,2-Tetrachloroethylsulfenyl chloride → HCID 12894656, 화합물

HRID 1706657
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HRID 1706657 반응식
[OH-].[Na+].[CH2:3]([NH:9][S:10]([CH2:13][CH2:14][CH3:15])(=[O:12])=[O:11])[CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[Cl:16][C:17]([Cl:23])([S:21]Cl)[CH:18]([Cl:20])[Cl:19]>ClCCl>[CH2:3]([N:9]([S:21][C:17]([Cl:23])([Cl:16])[CH:18]([Cl:20])[Cl:19])[S:10]([CH2:13][CH2:14][CH3:15])(=[O:12])=[O:11])[CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 144531,1,2,2-Tetrachloroethylsulfenyl chlorideHCID 14798Sodium HydroxideHCID 12894655N-Hexyl-1-propanesulfonamide

생성물 1

HCID 12894656HCID 12894656, 화합물수율 40.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

A 3.8 g (0.047 mol) sample of 50% weight aqueous sodium hydroxide solution was added dropwise to a cooled (8° C.) solution of 9.0 g (0.043 mol) N-hexyl propanesulfonamide and 11.0 g (0.047 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride in 150 ml dichloromethane. After the addition was completed, the reaction was stirred at about 25° C. for 4 hours during which time a precipitate formed. The reaction mixture was then washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give an oily residue. The residue was chromatographed through 250 g silica gel with 10% ethylether/90% hexane elution to give 7 g of the product as a yellow oil. The elemental analysis for the product showed: %S, calc. 15.8, found 16.2; %Cl, calc. 35.0, found 33.5. The product is tabulated in Table I as Compound No. 1.

후처리

  1. additionAfter the addition
  2. customformed
  3. washThe reaction mixture was then washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customto give an oily residue
  7. customThe residue was chromatographed through 250 g silica gel with 10% ethylether/90% hexane elution

출처 및 근거

ORD 기록
ord-26d4e09c2c18459caf5708ff4222bb5a
출처 데이터셋
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04208348

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