ChemicalBook CAS DataBase List 2',4',6'-Trihydroxyacetophenone monohydrate

2',4',6'-Trihydroxyacetophenone monohydrate synthesis

12synthesis methods

Product Name:2',4',6'-Trihydroxyacetophenone monohydrate
CAS Number:480-66-0
Molecular formula:C8H8O4
Molecular Weight:168.15

Preparation by reaction of acetic anhydride on phloroglucinol,
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%).

108-73-6
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75-05-8 Synthesis

75-05-8
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2',4',6'-Trihydroxyacetophenone monohydrate

480-66-0
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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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108-73-6
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$13.00/5g

75-36-5 Synthesis