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Methanesulfonyl chloride → HCID 13655348, 화합물

HRID 745277
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HRID 745277 반응식
[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]
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참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 13655347HCID 13655347, 화합물

생성물 1

HCID 13655348HCID 13655348, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b57e9eeabebb423aac11900eb6ad1fef
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04598085

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