1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 19848625、化合物

HRID 1608195ノート

反応式

HRID 1608195 の反応式
[NH2:1][CH2:2][CH:3]1[O:8][CH:7]([CH3:9])[CH2:6][N:5]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[CH2:4]1.[NH2:18][C:19]1[C:27]([Cl:28])=[CH:26][C:22]([C:23](O)=[O:24])=[C:21]([O:29][CH2:30][CH3:31])[CH:20]=1.Cl.C(N=C=NCCCN(C)C)C>ClCCl>[NH2:18][C:19]1[C:27]([Cl:28])=[CH:26][C:22]([C:23]([NH:1][CH2:2][CH:3]2[O:8][CH:7]([CH3:9])[CH2:6][N:5]([CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[CH2:4]2)=[O:24])=[C:21]([O:29][CH2:30][CH3:31])[CH:20]=1

参加物

5

反応物 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 10037975HCID 10037975、化合物HCID 105366584-Amino-5-chloro-2-ethoxybenzoic acid

生成物 1

HCID 19848625HCID 19848625、化合物収率 66.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

To a solution of 2-aminomethyl-4-(2-chlorobenzyl)-6-methylmorpholine (2.2 g) in dichloromethane (50 ml), 4-amino-5-chloro-2-ethoxybenzoic acid (1.9 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.7 g) are added. The reaction mixture is stirred at 25° C. for 4 hours, washed successively with water, aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is chromatographed on silica gel with ethyl acetate-hexanechloroform (1:1:1) to give the title compound (2.6 g) as an oil.

後処理

  1. washwashed successively with water, aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulfate
  3. distillationThe solvent is distilled off under reduced pressure
  4. customthe residue is chromatographed on silica gel with ethyl acetate-hexanechloroform (1:1:1)

出典と根拠

ORDレコード
ord-95de7eb35e774e099fd55593746543c0
出典データセット
uspto-grants-1989_09
特許番号
US04870074

反応ノート

読み込み中…