Diiodomethane → 12H-dibenzo[d,g][1,3]dioxocin-12-one

温度

105 °C

2,2'-Dihydroxybenzophenone (10.0 g, 46.7 mmol) and diiodomethane (13.1 g, 49 mmol) was dissolved in dry N,N-dimethylformamide (180 ml). Dried finely powdered potassium carbonate (9.2 g, 66.7 mmol) was added and the mixture was heated at 105° C. for 16 h. After cooling to room temperature the reaction mixture was poured into ice water (500 ml). The precipitate was collected by filtration after 0.5 h, washed with water on the filter and dissolved in a mixture of ethanol (80 ml) and 4 N sodium hydroxide (20 ml). The solution was stirred at reflux temperature for 1 h, cooled and diluted with water (300 ml). The formed crystalline precipitate was filtered off, washed with water (50 ml) and dried in vacuo, affording 12H-dibenzo[d,g][1,3]dioxocin-12-one as a solid (9.5 g, 90%).

1. additionwas added
2. temperatureAfter cooling to room temperature the reaction mixture
3. filtrationThe precipitate was collected by filtration after 0.5 h
4. washwashed with water on the
5. filtrationfilter
6. dissolutiondissolved in a mixture of ethanol (80 ml) and 4 N sodium hydroxide (20 ml)
7. temperatureat reflux temperature for 1 h
8. temperaturecooled
9. additiondiluted with water (300 ml)
10. filtrationThe formed crystalline precipitate was filtered off
11. washwashed with water (50 ml)
12. customdried in vacuo

ORDレコード

ord-8e513a295b2b4f92849110bcc7334102

出典データセット

uspto-grants-1999_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05916889