تفاعل #4625

ord-75fb8b38e64d40b591e7fff45e062a05

معادلة التفاعل

c1ccc(COc2ccc(OCC3CO3)cc2)cc1
benzyl [4-(2,3-epoxypropoxy)phenyl]ether
CC(COc1ccc2c(c1)C(=O)NC(C)(C)O2)NCc1ccccc1
6-(2-benzylaminopropoxy)-2,3-dihydro-2,2-dimethyl-4H-1,3-benzoxazin-4-one
CC(COc1ccc2c(c1)C(=O)NC(C)(C)O2)N(Cc1ccccc1)CC(O)COc1ccc(OCc2ccccc2)cc1
1-[N-[2-(2,3-dihydro-2,2-dimethyl-4-oxo-4H-1,3-benzoxazin-6-yloxy)-1-methylethyl]benzylamino]-3-(4-benzyloxyphenoxy)propan-2-ol

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحfiltered
  2. 2
    تركيزconcentrated by evaporation

الإجراء التجريبي

A solution of 15.4 g of benzyl [4-(2,3-epoxypropoxy)phenyl]ether and 17.0 g of 6-(2-benzylaminopropoxy)-2,3-dihydro-2,2-dimethyl-4H-1,3-benzoxazin-4-one in 100 ml of isopropanol is refluxed for 24 hours, filtered and concentrated by evaporation. Trituration of the residue with approximately 200 ml of ether results in crystallisation of 1-[N-[2-(2,3-dihydro-2,2-dimethyl-4-oxo-4H-1,3-benzoxazin-6-yloxy)-1-methylethyl]benzylamino]-3-(4-benzyloxyphenoxy)propan-2-ol having a melting point of 149°-160° (in which the enantiomer pair A is present in greater amount).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727067uspto-grants-1988_02