Trifluoroacetic anhydride → 2-Bromo-4-fluorobenzonitrile
반응식
[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=O.FC(F)(F)C(OC(=O)C(F)(F)F)=O>N1C=CC=CC=1>[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]#[N:6]참가 물질
4
실험 절차
A solution of 10.9 g. (0.05 mole) of 2-bromo-4-fluorobenzamide in 50 ml. of dry pyridine is stirred and cooled in an ice-bath while 11.2 g. (0.0525 mole) of trifluoroacetic anhydride is added dropwise. After 2 hours at room temperature, the bulk of the solvent is evaporated under reduced pressure and the residue is dissolved in ether. Evaporation of the washed and dried ethereal extract under reduced pressure leaves the product as the residual solid. Sublimation at 55° C. and 0.05 mm. yields white crystals, m.p. 75°-76.5° C. A sample from a previous experiment was resublimed for analysis, m.p. 77°-78° C.
후처리
- temperaturecooled in an ice-bath while 11.2 g
- customthe bulk of the solvent is evaporated under reduced pressure
- dissolutionthe residue is dissolved in ether
- customEvaporation of the
- washwashed
- customdried ethereal
- extractionextract under reduced pressure
- customleaves the product as the residual solid
- customat 55° C.
- customyields white crystals, m.p. 75°-76.5° C
출처 및 근거
- ORD 기록
- ord-af1a3cbda2d341cd86e5068c19029d57
- 출처 데이터셋
- uspto-grants-1978_01
- 특허 번호
- US04071570
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