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Dicyclohexylcarbodiimide → 4-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide

HRID 1926592
ノート
印刷プレビュー

反応式

HRID 1926592 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([OH:15])=O)=[CH:11][CH:10]=2)[CH2:4][CH2:3]1.C1(N=C=NC2CCCCC2)CCCCC1.[NH2:33][C:34]1[CH:35]=[C:36]([NH:41][C:42]2[N:47]=[C:46]([C:48]3[CH:49]=[N:50][CH:51]=[CH:52][CH:53]=3)[CH:45]=[CH:44][N:43]=2)[C:37]([CH3:40])=[N:38][CH:39]=1>C(Cl)Cl>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([C:13]([NH:33][C:34]3[CH:39]=[N:38][C:37]([CH3:40])=[C:36]([NH:41][C:42]4[N:47]=[C:46]([C:48]5[CH:49]=[N:50][CH:51]=[CH:52][CH:53]=5)[CH:45]=[CH:44][N:43]=4)[CH:35]=3)=[O:15])=[CH:16][CH:17]=2)[CH2:6][CH2:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 47697824-(4-Methyl-1-piperazinylmethyl)benzoic acidHCID 469098562-Methyl-N3-(4-(pyridin-3-yl)pyriMidin-2-yl)pyridine-3,5-diaMine

生成物 1

HCID 692278004-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide収率 75%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a flask was added 4-((4-methylpiperazin-1-yl)methyl)benzoic acid (3.2 g), dicyclohexylcarbodiimide (3.0 g), N-(5-amino-2-methylpyridin-3-yl)-4-(3-pyridyl)pyrimidin-2-amine (3.0 g) and CH2Cl2 (100 mL) and the reaction mixture was stirred at room temperature overnight. The reaction mixture was filtrated and the filtrate was washed with water (100 mL×2), dried, filtrated, concentrated, and purified through column chromatography to give 4-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide (4.0 g).

後処理

  1. filtrationThe reaction mixture was filtrated
  2. washthe filtrate was washed with water (100 mL×2)
  3. customdried
  4. filtrationfiltrated
  5. concentrationconcentrated
  6. custompurified through column chromatography

出典と根拠

ORDレコード
ord-0b3883f5078e4a63a80a15da31216315
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08183242B2

反応ノート

読み込み中…

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