Aniline → Aniline;2-bromoethylphosphonic acid
반응식
C([O:3][P:4]([CH2:9][CH2:10][Br:11])(=[O:8])[O:5]CC)C.[NH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>Br.C(O)C>[C:13]1([NH2:12])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[Br:11][CH2:10][CH2:9][P:4](=[O:3])([OH:8])[OH:5]참가 물질
5
실험 절차
A solution of about 50 g of diethyl-2-bromoethyl-phosphonate in about 255 ml of about 48% hydrobromic acid was kept at reflux (about 95°-100° C.) overnight. The solvent was removed under reduced pressure and the residue evaporated twice with toluene, giving a syrup. This syrup was dissolved in about 65 ml of about 99% ethanol, about 20 g of aniline was added dropwise and the solid was collected, washed with cold about 99% ethanol (at about 0° C.) and dried in vacuo, giving about 30.6 g of the desired reagent, mp 157°-158° C.
후처리
- temperatureat reflux (about 95°-100° C.) overnight
- customThe solvent was removed under reduced pressure
- customthe residue evaporated twice with toluene
- customgiving a syrup
- customthe solid was collected
- washwashed with cold about 99% ethanol (at about 0° C.)
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-5d1e1bdf5d674b32b63e5a0ec0e63fca
- 출처 데이터셋
- uspto-grants-1987_02
- 특허 번호
- US04640913
반응 노트
불러오는 중…