반응 #1052049

ord-943e695952cf4cab8fbdceea88c46fd9

반응 방정식

O=C1OC(=O)c2c(F)c(F)c(F)c(F)c21
Tetrafluorophthalic anhydride
CN(C)C=O
N,N-dimethylformamide
c1ccncc1
pyridine
NN
hydrazine
NNC(=O)c1c(F)c(F)c(F)c(F)c1C(=O)NN
Compound 43
수율 87.0%
NNC(=O)c1c(F)c(F)c(F)c(F)c1C(=O)NN
tetrafluorophthalhydrazide
수율 87.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture is concentrated in vacuo
  2. 2
    workup.ADDITIONthe residue is poured into water (200 mL)
  3. 3
    기타The precipitate formed
  4. 4
    여과is collected by filtration
  5. 5
    세척washed with water
  6. 6
    기타air-dried

실험 절차

Tetrafluorophthalic anhydride (400 mg, 1.8 mmol) is dissolved in 10 mL of anhydrous N,N-dimethylformamide (DMF) that contains anhydrous pyridine (0.47 mL, 5.8 mmol). To the solution is slowly added hydrazine (64 mg, 2.0 mmol). The resulting mixture is stirred overnight. The reaction mixture is concentrated in vacuo, and the residue is poured into water (200 mL). The precipitate formed is collected by filtration, washed with water and air-dried to give Compound 43 (369 mg, yield: 87%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05773236uspto-grants-1998_06