Acetic Anhydride → 6-Hydroxy-2-naphthone

温度

-50 °C

These examples further illustrate the process of the invention. In each of the examples, a 300 cc Hastelloy C autoclave was charged with a quantity of 2-naphthyl acetate. In Examples 7, 8 and 9, one mole of acetic anhydride per mole of 2-naphthyl acetate was also charged with the 2-naphthyl acetate. The autoclave was cooled to -50° C. and evacuated to 150 mm Hg whereupon a quantity of anhydrous hydrogen fluoride was transferred from a cylinder to the autoclave at such a rate that the temperature did not exceed 0° C. The contents were warmed to reaction temperature and stirred for a predetermined period of reaction during which time a pressure of ca. 40 psig was generated. At the end of the run, the hydrogen fluoride was vented through a caustic scrubber and the contents of the autoclave were poured onto ca. 30 g of ice. The pH of the mixture was adjusted to 6.5 using a solution of 50% potassium hydroxide and the mixture was then extracted with 75 mL of ethyl acetate (3×). The organic solution was dried over anhydrous MgSO4, filtered, and the solvent was removed using a rotary evaporator to yield the 6-hydroxy-2-naphthone.

1. customevacuated to 150 mm Hg whereupon a quantity of anhydrous hydrogen fluoride
2. customdid not exceed 0° C
3. temperatureThe contents were warmed to reaction temperature
4. additionthe contents of the autoclave were poured onto ca. 30 g of ice
5. extractionthe mixture was then extracted with 75 mL of ethyl acetate (3×)
6. dry with materialThe organic solution was dried over anhydrous MgSO4
7. filtrationfiltered
8. customthe solvent was removed
9. customa rotary evaporator

ORDレコード

ord-9baaafb34a7a45d39f17da0b6fe58052

出典データセット

uspto-grants-1987_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04675449