Sodium methanesulfinate → 5-methanesulfonylmethyl-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone

HRID 259009노트

반응식

HRID 259009 반응식
Cl[CH2:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH2:7][C:8]2=[O:14].[CH3:15][S:16]([O-:18])=[O:17].[Na+]>C(O)C>[CH3:15][S:16]([CH2:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH2:7][C:8]2=[O:14])(=[O:18])=[O:17]

참가 물질

4

반응물 2

HCID 2733271Sodium methanesulfinateHCID 123936195-(chloromethyl)-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone

생성물 1

HCID 132865845-methanesulfonylmethyl-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 100 ml. of ethanol are added 10 g. of 5-chloromethyl-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone and 5.4 g. of sodium methanesulfinate, and the mixture is heated on reflux for 2 hours. Then, the reaction mixture is concentrated and the residue is dissolved in chloroform and washed with water. The chloroform layer is dried in the conventional manner and the chloroform is distilled off. The procedure provides 5-methanesulfonylmethyl-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone melting at 225° -230° C(decomp.).

후처리

  1. temperatureon reflux for 2 hours
  2. concentrationThen, the reaction mixture is concentrated
  3. dissolutionthe residue is dissolved in chloroform
  4. washwashed with water
  5. dry with materialThe chloroform layer is dried in the conventional manner
  6. distillationthe chloroform is distilled off

출처 및 근거

ORD 기록
ord-18d17fd6f9784ef5a59d3cfd35256d89
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035512

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