Acetonitrile → HCID 68125252、化合物

HRID 259607

反応式

HRID 259607 の反応式
[CH3:1][O:2][C:3]([NH:5][CH:6]=[CH:7][C:8]1[CH:18]=[CH:17][C:11]([O:12][CH2:13][CH:14]2[O:16][CH2:15]2)=[CH:10][CH:9]=1)=[O:4].N[CH:20]([CH3:29])[CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(#[N:32])C>>[CH3:1][O:2][C:3]([NH:5][CH:6]=[CH:7][C:8]1[CH:18]=[CH:17][C:11]([O:12][CH:13]([NH2:32])[CH:14]([OH:16])[CH2:15][CH:20]([CH3:29])[CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[CH:10][CH:9]=1)=[O:4]

参加物

4

反応物 3

HCID 6342Acetonitrile2 回HCID 311601-Methyl-3-phenylpropylamineHCID 54361820HCID 54361820、化合物

生成物 1

HCID 68125252HCID 68125252、化合物

実験手順

2.49 g (0.01 mol) of 1-[p-(2-methoxycarbonylaminovinyl)-phenoxy]-2,3-epoxy-propane are dissolved in 25 ml of acetonitrile and added dropwise to a boiling stirred solution of 1.42 g (0.0095 mol) of 3-amino-1-phenylbutane in 20 ml of acetonitrile. The mixture is stirred for 20 hours under reflux, the solvent is removed by distillation under reduced pressure and the oil which remains is partitioned between 120 ml of 0.1 N hydrochloric acid and 100 ml of ethyl acetate. The hydrochloric acid extract is separated off, rendered alkaline with sodium carbonate and extracted four times with 50 ml of ethyl acetate at a time. The organic phases are dried over sodium sulphate and evaporated in vacuo. The resulting oil yields 1-[p-(2-methoxycarbonylaminovinyl)-phenoxy]-2-hydroxy-3-(1-methyl-3-phenyl-propyl)-amino propane of melting point 126°-127° C., from ethyl acetate.

後処理

  1. additionadded dropwise to a boiling
  2. temperatureunder reflux
  3. customthe solvent is removed by distillation under reduced pressure
  4. customthe oil which remains is partitioned between 120 ml of 0.1 N hydrochloric acid and 100 ml of ethyl acetate
  5. extractionThe hydrochloric acid extract
  6. customis separated off
  7. extractionextracted four times with 50 ml of ethyl acetate at a time
  8. dry with materialThe organic phases are dried over sodium sulphate
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-ef3648c84c35470190270878127e25e2
出典データセット
uspto-grants-1977_07
特許番号
US04038414

関連ノート

読み込み中…