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

HRID 259009ノート

反応式

HRID 259009 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-18d17fd6f9784ef5a59d3cfd35256d89
出典データセット
uspto-grants-1977_07
特許番号
US04035512

反応ノート

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