5-(4-Chlorobenzyl)-2-methylthiopyrimid-4-one → 2-[3-(N-ethyl-N-pyrid-2-ylamino)propylamino]-5-(4-chlorobenzyl)pyrimid-4-one

HRID 464372노트

반응식

HRID 464372 반응식
[C:1]1([N:7]([CH2:14][CH2:15][CH2:16][N:17]2[C:21](=O)C3=CC=CC=C3C2=O)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:6]=CC=CC=1.CSC1[NH:35][C:34](=[O:36])[C:33]([CH2:37][C:38]2[CH:43]=[CH:42][C:41]([Cl:44])=[CH:40][CH:39]=2)=[CH:32][N:31]=1>N1C=CC=CC=1>[CH2:1]([N:7]([CH2:14][CH2:15][CH2:16][NH:17][C:21]1[NH:35][C:34](=[O:36])[C:33]([CH2:37][C:38]2[CH:39]=[CH:40][C:41]([Cl:44])=[CH:42][CH:43]=2)=[CH:32][N:31]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=1)[CH3:6]

참가 물질

4

반응물 2

HCID 129459805-(4-Chlorobenzyl)-2-methylthiopyrimid-4-oneHCID 20186606N-[3-(N-phenyl-N-pyrid-2-ylamino)propyl]phthalimide

생성물 1

HCID 202628722-[3-(N-ethyl-N-pyrid-2-ylamino)propylamino]-5-(4-chlorobenzyl)pyrimid-4-one

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Substituting ethyl iodide (10.31 g) for n-propyl iodide and using the corresponding molar proportions of the other reagents in the method of example 15(i) gave 2-[N-(3-aminopropyl)-N-ethylamino]pyridine (2.32 g) as an oil. (ii) 2-[N-(3-aminopropyl)-N-ethylamino]pyridine (1.0 g) and 2-methylthio-5-(4-chlorobenzyl)pyrimid-4-one (0.99 g) were heated together under reflux in pyridine (2.5 ml) for 28 hr. After stripping the residue was crystallized from ethanol and recrystallized from ethanol/water to give 2-[3-(N-ethyl-N-pyrid-2-ylamino)propylamino]-5-(4-chlorobenzyl)pyrimid-4-one 0.9 H2O, 1.23 g (79%) m.p. 86°-89° C.

후처리

  1. customwas crystallized from ethanol
  2. customrecrystallized from ethanol/water

출처 및 근거

ORD 기록
ord-e2aafc5e01d348079ff4ff9e844c806b
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04547506

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