تفاعل #83054

ord-d0a0fd2d1d4e4ea6aa4e79b55d1e6f4c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىArgon is bubbled through the reaction
  2. 2
    أخرىto remove the excess phosgene
  3. 3
    أخرىthe solvents are removed under house vacuum
  4. 4
    workup.DISSOLUTIONThe resulting oil is dissolved in 14 ml of ethyl alcohol
  5. 5
    workup.ADDITIONdiluted with 14 ml of petroleum ether
  6. 6
    أخرىThe formed crystals are collected
  7. 7
    أخرىdried

الإجراء التجريبي

A suspension of 1.752 g of DL-2-aminopimelic acid, 55 ml of tetrahydrofuran and 16 ml of 1.93M phosgene in toluene is heated, in an oil bath, at 50° C. for 1 hour. Argon is bubbled through the reaction to remove the excess phosgene and the solvents are removed under house vacuum. The resulting oil is dissolved in 14 ml of ethyl alcohol, diluted with 14 ml of petroleum ether and the solution stored overnight at room temperature. The formed crystals are collected and dried to give 1.6 g of the desired product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05623081uspto-grants-1997_04