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Methanesulfonyl chloride → HCID 13655348、化合物

HRID 745277
ノート
印刷プレビュー

反応式

HRID 745277 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([CH2:12][CH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)[CH2:10][OH:11].[CH3:19][S:20](Cl)(=[O:22])=[O:21]>N1C=CC=CC=1>[CH3:19][S:20]([O:11][CH2:10][CH:9]([C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1])[CH2:12][CH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)(=[O:22])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 13655347HCID 13655347、化合物

生成物 1

HCID 13655348HCID 13655348、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirred and cooled (ice-bath) mixture of 22 parts of 2,4-dichloro-β-(cyclohexylmethyl)benzeneethanol and 50 parts of pyridine are added dropwise 8.8 parts of methanesulfonyl chloride. Upon completion, stirring is continued for 3 hours at room temperature. The reaction mixture is poured onto water and the product is extracted twice with trichloromethane. The combined extracts are washed twice with a diluted hydrochloric acid solution and once with water, dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane, yielding 16.5 parts of 3-cyclohexyl-2-(2,4-dichlorophenyl)propyl methanesulfonate; mp. 105.1° C.

後処理

  1. temperaturecooled
  2. stirringUpon completion, stirring
  3. additionThe reaction mixture is poured onto water
  4. extractionthe product is extracted twice with trichloromethane
  5. washThe combined extracts are washed twice with a diluted hydrochloric acid solution and once with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is crystallized from 2,2'-oxybispropane

出典と根拠

ORDレコード
ord-b57e9eeabebb423aac11900eb6ad1fef
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04598085

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート