Sodium Hydroxide → 5-(Benzyloxy)-2-sulfanylphenol

HRID 322946ノート

反応式

HRID 322946 の反応式
[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:12]2[S:13]C(=O)[O:15][C:11]=2[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:12]([SH:13])=[C:11]([OH:15])[CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 106826256-Benzyloxy-1,3-benzoxathiol-2-one

生成物 1

HCID 219047055-(Benzyloxy)-2-sulfanylphenol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 6-benzyloxy-1,3-benzoxathiol-2-one (35 g), aqueous sodium hydroxide solution (200 mL; 2 N) and methanol (50 mL) is stirred at ambient temperature for 16 hours and then it is heated at reflux for 30 minutes. The reaction mixture is then evaporated to dryness and the residue is acidified to pH 1 by treatment with concentrated hydrochloric acid (20 mL). The residue is diluted with water (200 mL) and then extracted with diethyl ether (3×200 mL). The combined organic extracts are washed with brine (100 mL), dried over magnesium sulphate, filtered and concentrated in vacuo, to give 5-benzyloxy-2-mercaptophenol, in the form of a yellow oil which solidified on standing overnight.

後処理

  1. temperatureit is heated
  2. temperatureat reflux for 30 minutes
  3. customThe reaction mixture is then evaporated to dryness
  4. additionThe residue is diluted with water (200 mL)
  5. extractionextracted with diethyl ether (3×200 mL)
  6. washThe combined organic extracts are washed with brine (100 mL)
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-88694364a4a04c1f8fba9618b2539281
出典データセット
uspto-grants-2001_04
特許番号
US06211234B1

反応ノート

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