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Diisopropylethylamine → HCID 59381877, 화합물

HRID 2355097
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HRID 2355097 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:31])=[C:6]([CH:30]=1)[C:7]([NH:9][C:10]1[CH:11]=[N:12][C:13]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([N:23]3[CH2:28][CH2:27][N:26]([CH3:29])[CH2:25][CH2:24]3)=[CH:19][CH:18]=2)=[N:14][CH:15]=1)=[O:8].C(N(C(C)C)CC)(C)C.[C:41](Cl)(=[O:52])[O:42][C:43]1[C:48]([CH3:49])=[CH:47][C:46]([CH3:50])=[CH:45][C:44]=1[CH3:51]>CN(C)C1C=CN=CC=1.ClCCl>[CH3:31][C:5]1[CH:4]=[CH:3][C:2]([NH:1][C:41](=[O:52])[O:42][C:43]2[C:48]([CH3:49])=[CH:47][C:46]([CH3:50])=[CH:45][C:44]=2[CH3:51])=[CH:30][C:6]=1[C:7](=[O:8])[NH:9][C:10]1[CH:11]=[N:12][C:13]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([N:23]3[CH2:24][CH2:25][N:26]([CH3:29])[CH2:27][CH2:28]3)=[CH:19][CH:18]=2)=[N:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 11106338HCID 11106338, 화합물HCID 16118190HCID 16118190, 화합물

생성물 1

HCID 59381877HCID 59381877, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

A 16×100 mm vial was charged with 5-amino-2-methyl-N-(2-(4-(4-methylpiperazin-1-yl)phenylamino)pyrimidin-5-yl)benzamide 30 (0.100 g, 0.24 mmol), 4-(dimethylamino)pyridine (0.0059 g, 0.048 mmol), dichloromethane (2 mL), and diisopropylethylamine (0.050 ml, 0.29 mmol). A solution of mesityl carbonochloridate (0.048 g, 0.24 mmol) in dichloromethane (1 mL) was added dropwise and the reaction mixture stirred at room temperature for 20 hours. The reaction mixture was purified via column chromatography on silica gel (gradient elution with 0 to 20% methanol in dichloromethane) to afford mesityl 4-methyl-3-((2-(4-(4-methylpiperazin-1-yl)phenylamino)pyrimidin-5-yl)carbamoyl)phenylcarbamate 47 as a bright yellow solid.

후처리

  1. customThe reaction mixture was purified via column chromatography on silica gel (gradient elution with 0 to 20% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-b43fec4a1e6d46dea06adf94ee4f5db6
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754717B2

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