반응 #52166

ord-82bcd2e31e4742e288da7ae9c3316792

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The residue was concentrated in vacuo
  2. 2
    기타the crude 3,5-dichloropyridine-4-carboxylic acid chloride was used in Step E without further purification

실험 절차

3,5-Dichloropyridine-4-carboxylic acid (0.5 g, 2.6 mmol; Reference Example 1) was dissolved in CH2Cl2 (1.75 mL) and DMF (50 μL). Thionyl chloride (0.21 mL, 2.86 mL) was added and the reaction mixture was heated at 50° C. for 20 h. The residue was concentrated in vacuo. The formation of the acid chloride was observed by TLC (50% EtOAc/hexane) and the crude 3,5-dichloropyridine-4-carboxylic acid chloride was used in Step E without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855708B2uspto-grants-2005_02