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

HRID 1589715ノート

反応式

HRID 1589715 の反応式
[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]

参加物

3

反応物 2

HCID 7853AllylamineHCID 155294Fluazifop-methyl

生成物 1

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

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0b5d0fcbd1944a6bbe83be6dfbb0c587
出典データセット
uspto-grants-1993_04
特許番号
US05199970

反応ノート

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