Diethyl 4-(trifluoromethyl)benzylphosphonate → {[4-(Trifluoromethyl)phenyl]methyl}phosphonic acid

HRID 1463570노트

반응식

HRID 1463570 반응식
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:17]=[CH:16][C:6]([CH2:7][P:8](=[O:15])([O:12]CC)[O:9]CC)=[CH:5][CH:4]=1>Cl.CCO>[F:19][C:2]([F:1])([F:18])[C:3]1[CH:17]=[CH:16][C:6]([CH2:7][P:8](=[O:9])([OH:12])[OH:15])=[CH:5][CH:4]=1

참가 물질

4

반응물 1

HCID 15819199Diethyl 4-(trifluoromethyl)benzylphosphonate

생성물 1

HCID 15818094{[4-(Trifluoromethyl)phenyl]methyl}phosphonic acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

The diethyl 4-trifluoromethylbenzylphosphonate (3.0 g, 10 mmol) was dissolved in a mixture of 50 mL of conc hydrochloric acid and 5 mL of EtOH and heated at reflux for 17 hours. After cooling the mixture in an ice bath, white crystalline material was collected. Recrystallization of the solid from H2O gave 1.80 g, 75% of the analytically pure product: mp=163°-164° C.; D.C.I.M.S.[MH+,241].

후처리

  1. temperatureheated
  2. temperatureat reflux for 17 hours
  3. temperatureAfter cooling the mixture in an ice bath
  4. customwhite crystalline material was collected
  5. customRecrystallization of the solid from H2O
  6. customgave 1.80 g, 75% of the analytically pure product

출처 및 근거

ORD 기록
ord-ea7351dfea5444b891650cde59aff8a0
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05300687

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