Metoclopramide → HCID 13140663, 화합물

HRID 614807

반응식

HRID 614807 반응식
[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[CH:12]=[C:13]([Cl:20])[C:14]([NH2:19])=[CH:15][C:16]=1[O:17][CH3:18])=[O:10])[CH2:4][CH3:5].C(N(CC)CC)C.[Cl:28][C:29]1[CH:41]=[CH:40][C:32]([O:33][C:34]([CH3:39])([CH3:38])[C:35](Cl)=[O:36])=[CH:31][CH:30]=1.[OH-].[Na+]>O.C(Cl)(Cl)Cl>[Cl:28][C:29]1[CH:41]=[CH:40][C:32]([O:33][C:34]([CH3:38])([CH3:39])[C:35]([NH:19][C:14]2[C:13]([Cl:20])=[CH:12][C:11]([C:9]([NH:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])=[O:10])=[C:16]([O:17][CH3:18])[CH:15]=2)=[O:36])=[CH:31][CH:30]=1

참가 물질

7

반응물 4

HCID 4168MetoclopramideHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 27813122-(4-Chlorophenoxy)-2-methylpropanoyl chloride

생성물 1

HCID 13140663HCID 13140663, 화합물수율 73.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

Metoclopramide (59.8 g.; 0.2 mole) and triethylamine (30.0 g; 0.3 mole) are dissolved in 400 ml. of chloroform. To this mixture there is added dropwise 2-(4-chlorphenoxy)-2-methylpropionic acid chloride (72.0 g.; 0.3 mole). The mixture is heated under reflux for two hours and is subsequently mixed with 100 ml. of 20% caustic soda solution and with water. After evaporation, the distillation residue is recrystallized from methanol whereby 73.2 g. (73.7% of theory) of 4-[2-(4-chlorphenoxy)isobutyroylamino]-5-chloro-2-methoxy-N-[2-(diethylamino)-ethyl]benzamide having a melting point of 120°-121° C. is obtained.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for two hours
  3. additionis subsequently mixed with 100 ml
  4. customAfter evaporation
  5. customthe distillation residue is recrystallized from methanol whereby 73.2 g

출처 및 근거

ORD 기록
ord-13329d2adcd34b1faab2c6dff917845c
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04146637

연결된 노트

불러오는 중…