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Water → 3-(2,2-Dimethoxyethylthio)phenol

HRID 972115
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HRID 972115 반응식
[SH:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.Cl[CH2:10][CH:11]([O:14][CH3:15])[O:12][CH3:13].O.[Cl-].[NH4+]>CN(C)C=O>[CH3:13][O:12][CH:11]([O:14][CH3:15])[CH2:10][S:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 609862-Chloro-1,1-dimethoxyethaneHCID 27366133-Hydroxybenzenethiol

생성물 1

HCID 203966733-(2,2-Dimethoxyethylthio)phenol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The S-sodium salt of 3-mercaptophenol prepared in Example 7 was dissolved in dimethylformamide (25 ml) and charged under nitrogen gas into a glass reaction vessel equipped with a mechanical stirrer, thermometer and addition funnel. The solution was heated to a temperature of 45 to 50° C., and 1-chloro-2,2-dimethoxyethane (3.15 grams) was added with stirring. After the addition was completed, stirring was continued for a period of about 3 hours. After this time the reaction mixture was poured into water (150 ml), and the resulting mixture was carefully neutralized with ammonium chloride. The mixture was then extracted with chloroform and the organic phase was separated. The organic portion was washed with water and then dried with phase separation paper. The dried solution was then stripped of solvent, leaving an oil. This oil was distilled, and the fraction boiling at 138° to 144° C. at 0.04 mm of Hg pressure was collected to yield the desired product 3-(2,2-dimethoxyethylthio)phenol.

후처리

  1. additioncharged under nitrogen gas into a glass reaction vessel
  2. customequipped with a mechanical stirrer
  3. additionthermometer and addition funnel
  4. additionwas added
  5. additionAfter the addition
  6. stirringstirring
  7. extractionThe mixture was then extracted with chloroform
  8. customthe organic phase was separated
  9. washThe organic portion was washed with water
  10. customdried with phase separation paper
  11. customleaving an oil
  12. distillationThis oil was distilled
  13. customthe fraction boiling at 138° to 144° C. at 0.04 mm of Hg pressure was collected

출처 및 근거

ORD 기록
ord-fd9fc539c0e141e59168781fe68fe50d
출처 데이터셋
uspto-grants-1979_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04163112

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