Acetic Anhydride → 2-(2-Acetoxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

HRID 544664노트

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HRID 544664 반응식
[OH:1][CH2:2][CH2:3][S:4][C:5]1[S:6][C:7]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[N:9]=1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>>[C:26]([O:1][CH2:2][CH2:3][S:4][C:5]1[S:6][C:7]([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)=[C:8]([C:10]2[CH:11]=[CH:12][C:13]([O:16][CH3:17])=[CH:14][CH:15]=2)[N:9]=1)(=[O:28])[CH3:27]

참가 물질

3

실험 절차

5.0 g of 2-(2-hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole are suspended in 50 ml of acetic anhydride and, while stirring, the suspension is heated to the boil and refluxed for 15 minutes. The product is concentrated to dryness by evaporation under reduced pressure, two 30 ml portions of xylene are added, with concentration by evaporation being carried out again after each addition to remove traces of acetic anhydride, and the residue is dried under reduced pressure. 2-(2-Acetoxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole is obtained in the form of an oil, Rf =0.33 (silica gel toluene/ethyl acetate 10:1), IR-spectrum: νC=O =1730 cm-1 (CCl4).

후처리

  1. temperaturethe suspension is heated to the boil
  2. temperaturerefluxed for 15 minutes
  3. concentrationThe product is concentrated to dryness by evaporation under reduced pressure, two 30 ml portions of xylene
  4. additionare added, with concentration by evaporation
  5. additionafter each addition
  6. customto remove traces of acetic anhydride
  7. customthe residue is dried under reduced pressure

출처 및 근거

ORD 기록
ord-e477768b3a92435bbd60403c66f39988
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451471

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