반응 #157265

ord-13aa5ad1abcf4b738ee9dfdee5adc231

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도after cooling
  2. 2
    기타evaporated down
  3. 3
    추출The residue is extracted with dichloromethane and water
  4. 4
    기타the organic phase is dried
  5. 5
    기타evaporated to dryness
  6. 6
    기타The residue is crystallised with petroleum ether/ethyl acetate

실험 절차

1.25 g 2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidine are placed in 5 ml dimethylformamide, first 1.05 ml diisopropylethylamine, then 0.960 g 3-morpholin-4-ylmethyl-phenylamine (J. Med. Chem. 1990, 33, 327) are added. The reaction mixture is sf 20 hours at 60° C., then after cooling evaporated down. The residue is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness. The residue is crystallised with petroleum ether/ethyl acetate. 1.28 g of the product are obtained as a powder.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822474B2uspto-grants-2014_09