تفاعل #6831

ord-443e59999fd64eac976cc8d305d90497

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe aqueous layer was re-extracted with 50 mL more dichloromethane
  2. 2
    تجفيفthe combined organics were dried over sodium sulfate
  3. 3
    أخرىEvaporation of the solvent

الإجراء التجريبي

A solution of 2,6,6-trimethoxy-6,7,8,9-tetrahydro-5H-benzocycloheptene (387 mg) and p-toluenesulfonic acid monohydrate (31 mg) was stirred in 5 mL of 1:1 water:acetone. The mixture was diluted with 50 mL of dichloromethane and 50 mL of saturated sodium hydrogen carbonate. The aqueous layer was re-extracted with 50 mL more dichloromethane and the combined organics were dried over sodium sulfate. Evaporation of the solvent gave 250 mg of 2-methoxy-5,7,8,9-tetrahydro-benzocyclohepten-6-one, which was converted to 2-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ylamine by using Procedure X.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084154B2uspto-grants-2006_08