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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
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반응식

HRID 1926592 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0b3883f5078e4a63a80a15da31216315
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183242B2

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