反応 #1691232

ord-a1b9e7944a80437fa48ba75504f0b0b9

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Xylene was removed on a rotary evaporator
  2. 2
    workup.DISTILLATIONthe residue distilled
  3. 3
    その他to give 11.09 g of distillate, b0.5 130-160° C. which

実験手順

Following the procedure of Examples 1 or 2,7-Isopropyl-8,8-dimethyl-8,9-dihydro-7H-6,10-dioxabenzocyclononene-5,11-dione was prepared from a solution of 14.81 g (0.1 mole) of phthalic anhydride and 16.30 g (0.11 mole) of 2,2,4-trimethyl-1,3-pentanediol (TMPD) in 75 mL of xylene. The catalyst was 49.4 mg of FASCAT® 4100 catalyst. Xylene was removed on a rotary evaporator and the residue distilled to give 11.09 g of distillate, b0.5 130-160° C. which was found by vapor phase chromatography (vpc) to consist of 84% of 7-Isopropyl-8,8-dimethyl-8,9-dihydro-7H-6,10-dioxabenzocyclononene-5,11-dione (40% yield). The residue from this distillation weighed 17.65 g.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05990321uspto-grants-1999_11