1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 19848625, 화합물

HRID 1608195노트

반응식

HRID 1608195 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 19848625HCID 19848625, 화합물수율 66.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-95de7eb35e774e099fd55593746543c0
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04870074

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