4-Methylmorpholine → 9-{2-[2-(3-Hydroxymethyl-phenyl)-1-methyl-ethylamino]-pyrimidin-4-yl}-2-phenyl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one

HRID 1785430노트

반응식

HRID 1785430 반응식
CS([C:5]1[N:10]=[C:9]([N:11]2[C:16]3=[N:17][C:18]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[CH:19][C:20](=[O:21])[N:15]3[CH2:14][CH2:13][CH2:12]2)[CH:8]=[CH:7][N:6]=1)(=O)=O.[NH2:28][CH:29]([CH3:39])[CH2:30][C:31]1[CH:32]=[C:33]([CH2:37][OH:38])[CH:34]=[CH:35][CH:36]=1.CN1CCOCC1>ClCCl.C(OCC)(=O)C>[OH:38][CH2:37][C:33]1[CH:32]=[C:31]([CH2:30][CH:29]([NH:28][C:5]2[N:10]=[C:9]([N:11]3[C:16]4=[N:17][C:18]([C:22]5[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=5)=[CH:19][C:20](=[O:21])[N:15]4[CH2:14][CH2:13][CH2:12]3)[CH:8]=[CH:7][N:6]=2)[CH3:39])[CH:36]=[CH:35][CH:34]=1

참가 물질

6

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온도
100 °C

실험 절차

A mixture of 9-(2-methanesulfonyl-pyrimidin -4-yl)-2-phenyl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one (344 mg, 0.90 mmol), [3-(2-amino-propyl)-phenyl]-methanol (371 mg, 2.25 mmol), and N-methylmorpholine (8 mL) was heated to 100° C. for 20 h. Reaction was diluted with dichloromethane (15 mL) and ethyl acetate (40 mL), washed three times with water (50 mL) then saturated sodium chloride (10 mL). Organic dried over magnesium sulfate then concentrated to a oil under vacuum. Product purified on silica and isolated as a white solid. M+1=469.

후처리

  1. customReaction
  2. washwashed three times with water (50 mL)
  3. dry with materialOrganic dried over magnesium sulfate
  4. concentrationthen concentrated to a oil under vacuum
  5. customProduct purified on silica
  6. customisolated as a white solid

출처 및 근거

ORD 기록
ord-9d93330cbfb24dd48d5ecbd2a97476b6
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504403B2

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