Triethylamine → HCID 11327334, 화합물

HRID 2102414노트

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C([O:3][CH2:4][CH2:5][O:6][NH:7][C:8]([C:10]1[C:11]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][C:21]=2[F:27])=[CH:12][C:13]2[N:14]([CH:16]=[CH:17][N:18]=2)[N:15]=1)=[O:9])=C.BrC1C=CC(NC2C(C(O)=O)=NN3C=CN=C3C=2)=C(F)C=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.C(OCCON)=C.CCN(CC)CC>CC(N(C)C)=O.CCOC(C)=O>[OH:3][CH2:4][CH2:5][O:6][NH:7][C:8]([C:10]1[C:11]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][C:21]=2[F:27])=[CH:12][C:13]2[N:14]([CH:16]=[CH:17][N:18]=2)[N:15]=1)=[O:9]

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실험 절차

Preparation of 7-(4-bromo-2-fluorophenylamino)-imidazo[1,2-b]pyridazine-6-carboxylic acid (2-vinyloxyethoxy)-amide: A mixture of 7-(4-bromo-2-fluorophenylamino)-imidazo[1,2-b]pyridazine-6-carboxylic acid (1.00 equiv), EDCI (1.50 equivalents), and HOBt (1.50 equivalents) in DMA is stirred for 30 minutes at room temperature under N2. O-(2-vinyloxy-ethyl)-hydroxylamine (3.00 equivalents) is added followed by Et3N (2.50 equivalents). After the reaction mixture is stirred for 16 hours at room temperature, it is diluted with EtOAc and washed with saturated NH4Cl solution, saturated NaHCO3 solution and saturated NaCl. The organic layer is dried (Na2SO4) and concentrated under reduced pressure to yield the desired product. The product may be purified by flash column chromatography if further purification is necessary.

후처리

stirringAfter the reaction mixture is stirred for 16 hours at room temperature
washwashed with saturated NH4Cl solution, saturated NaHCO3 solution and saturated NaCl
dry with materialThe organic layer is dried (Na2SO4)
concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록: ord-5539dadd6eee48d693ed1ee674ed673b
출처 데이터셋: uspto-grants-2009_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07576072B2

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