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 1785430ノート

反応式

HRID 1785430 の反応式
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

参加物

6

反応物 3

HCID 79724-MethylmorpholineHCID 247215123-(2-Aminopropyl)benzyl alcoholHCID 575931249-(2-Methanesulfonyl-pyrimidin-4-yl)-2-phenyl-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one

生成物 1

HCID 575931789-{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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d93330cbfb24dd48d5ecbd2a97476b6
出典データセット
uspto-grants-2009_03
特許番号
US07504403B2

反応ノート

読み込み中…