2',4',6'-Trihydroxyacetophenone monohydrate synthesis
- Product Name:2',4',6'-Trihydroxyacetophenone monohydrate
- CAS Number:480-66-0
- Molecular formula:C8H8O4
- Molecular Weight:168.15
with concentrated sulfuric acid at 130° (70%)
with boron trifluoride at 10° (62.5–68%)
with zinc chloride at 145–150° (50%)
with Amberlite IR-120 or Zeokarb 225 (cation exchange resins, sulfonic acid type) at 160° (39%).
Yield:480-66-0 96.2%
Reaction Conditions:
Stage #1:3,5-dihydroxyphenol;acetonitrile with hydrogenchloride;zinc(II) chloride in di-isopropyl ether at 0;
Stage #2: with water for 2 h;Reflux;
Steps:
Phloroacetophenone (1)
A mixture of well-dried phloroglucinol(250 g, 1.98 mol), anhydrous acetonitrile (365 mL,6.95 mol), diisopropyl ether (838 mL, 5.95 mol) and finelypowdered fused zinc chloride (49.5 g, 0.036 mol) was cooledin an ice-salt mixture at 0 °C under stirring for 7 h, by passingdry HCl gas. The flask is allowed to cool in an ice-chest inrefrigerator for overnight. On decanting the diisopropyl ethera bulky orange-yellow precipitate was separated and washedthe precipitate with diisopropyl ether (100 mL). The solid wastransferred into a round bottom flask and added 2.5 L of distilledwater (2.5 L) and refluxed under stirring for 2 h at 120 °C. Themixture was cooled to room temperature and left overnight.Pale yellow needles were observed and the product was filteredand dried under vacuum oven at 120 °C. The yield was 96.2% with a purity of 99.9 % obtained.
References:
Rambabu;Kumari;Baby Ramana;Ramani;Subbaraju;Hari Babu [Asian Journal of Chemistry,2016,vol. 28,# 5,p. 1139 - 1143]
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![Ethanone, 1-[2,4,6-tris[[(1,1-dimethylethyl)dimethylsilyl]oxy]phenyl]-](/CAS/20210111/GIF/265975-36-8.gif)
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480-66-0
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