1-Hydroxybenzotriazole → N-(4-morpholin-4-ylbenzyl)-3-oxo-6-pyridin-4-yl-2,3-dihydropyridazine-4-carboxamide

HRID 970183

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[O:1]=[C:2]1[C:7]([C:8]([NH:10][CH2:11][CH2:12][C:13](OCC)=O)=[O:9])=[CH:6][C:5]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)=[N:4][NH:3]1.O=C1C(C(O)=O)=CC(C2C=CN=CC=2)=NN1.ON1C2C=CC=CC=2N=N1.[O:50]1[CH2:55][CH2:54][N:53]([C:56]2[CH:63]=CC(CN)=[CH:58][CH:57]=2)[CH2:52][CH2:51]1.C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1>CN(C)C=O>[N:53]1([C:56]2[CH:63]=[CH:13][C:12]([CH2:11][NH:10][C:8]([C:7]3[C:2](=[O:1])[NH:3][N:4]=[C:5]([C:18]4[CH:19]=[CH:20][N:21]=[CH:22][CH:23]=4)[CH:6]=3)=[O:9])=[CH:58][CH:57]=2)[CH2:54][CH2:55][O:50][CH2:51][CH2:52]1

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실험 절차

Working as in example 13 for the preparation of ethyl 3-[(3-oxo-6-pyridin-4-yl-2,3-dihydropyridazine-4-carbonyl)amino]propionate, but starting with 0.3 g of 3-oxo-6-pyridin-4-yl-2,3-dihydropyridazine-4-carboxylic acid, 30 cm3 of N,N-dimethylformamide, 0.233 g of 1-hydroxybenzotriazole, 0.265 g of 4-morpholinobenzylamine, 0.31 cm3 of N,N-diisopropylethylamine and 0.65 g of O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate, and after purification by chromatography on silica gel (particle size 40-63 μm, under an argon pressure of 150 kPa), eluting with dichloromethane, 0.13 g of N-(4-morpholin-4-ylbenzyl)-3-oxo-6-pyridin-4-yl-2,3-dihydropyridazine-4-carboxamide was obtained in the form of a yellow solid melting at 252° C.

후처리

customafter purification by chromatography on silica gel (particle size 40-63 μm
washunder an argon pressure of 150 kPa), eluting with dichloromethane

출처 및 근거

ORD 기록: ord-b7fa7a9656fe49ad9e36e80066d42dd0
출처 데이터셋: uspto-grants-2007_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07309701B2

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