تفاعل #2006473

ord-08b590fb32c34c1ab5e03c36feb43304

معادلة التفاعل

CC(C)(C)OP(=O)([O-])OC(C)(C)C
bis-tert butyl phosphate
ClCI
chloroiodomethane
CC(C)(C)OP(=O)(OCCl)OC(C)(C)C
di-tert-butyl chloromethyl phosphate

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe volatiles were removed in vacuo
  2. 2
    workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
  3. 3
    ترشيحwas filtered away
  4. 4
    أخرىConcentration of the filtrate and final removal of volatiles

الإجراء التجريبي

The tetrabutylammonium salt of bis-tert butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) were stirred at room temperature for four hours and then the volatiles were removed in vacuo. 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate and final removal of volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate (112 g), typically as a light yellow or brown oil, which was utilized in the next step without any further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08168615B2uspto-grants-2012_05