Allylamine → N-allyl-2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]-propionic acid amide

HRID 1589715노트

반응식

HRID 1589715 반응식
[F:1][C:2]([F:24])([F:23])[C:3]1[CH:4]=[CH:5][C:6]([O:9][C:10]2[CH:22]=[CH:21][C:13]([O:14][CH:15]([CH3:20])[C:16](OC)=[O:17])=[CH:12][CH:11]=2)=[N:7][CH:8]=1.[CH2:25]([NH2:28])[CH:26]=[CH2:27]>>[CH2:25]([NH:28][C:16](=[O:17])[CH:15]([O:14][C:13]1[CH:12]=[CH:11][C:10]([O:9][C:6]2[CH:5]=[CH:4][C:3]([C:2]([F:24])([F:23])[F:1])=[CH:8][N:7]=2)=[CH:22][CH:21]=1)[CH3:20])[CH:26]=[CH2:27]

참가 물질

3

반응물 2

HCID 7853AllylamineHCID 155294Fluazifop-methyl

생성물 1

HCID 53760130N-allyl-2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]-propionic acid amide

반응 조건

온도
60 °C

실험 절차

A mixture containing 11.85 g (0.035 mol) of methyl 2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]-propionate and 11.5 g (0.2 mol) of allylamine is boiled under reflux (about 60° C.) for 10 hours. (The reaction is followed by gas chromatography.) Thereafter, the excess of allylamine is distilled off and the residue is dissolved in benzene. After washing the solution cooled down with 5% aqueous hydrochloric acid and then with saturated sodium chloride solution, the organic phase is dried over anhydrous magnesium sulfate and evaporated. The crude product is recrystallized from petroleum ether (b.p. 120° C.) containing a small amount of toluene.

후처리

  1. distillation) Thereafter, the excess of allylamine is distilled off
  2. dissolutionthe residue is dissolved in benzene
  3. washAfter washing the solution
  4. temperaturecooled down with 5% aqueous hydrochloric acid
  5. dry with materialwith saturated sodium chloride solution, the organic phase is dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe crude product is recrystallized from petroleum ether (b.p. 120° C.)
  8. additioncontaining a small amount of toluene

출처 및 근거

ORD 기록
ord-0b5d0fcbd1944a6bbe83be6dfbb0c587
출처 데이터셋
uspto-grants-1993_04
특허 번호
US05199970

반응 노트

불러오는 중…