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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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1,1,2,2-Tetrachloroethylsulfenyl chloride → HCID 12894656、化合物

HRID 2287167
ノート
印刷プレビュー

反応式

HRID 2287167 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 12894656HCID 12894656、化合物収率 40.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b3aa4753d7a24f889195e7cd51d2eeb4
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04269856

反応ノート

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