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

HRID 322946노트

반응식

HRID 322946 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 219047055-(Benzyloxy)-2-sulfanylphenol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-88694364a4a04c1f8fba9618b2539281
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211234B1

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