Triethylamine → HCID 57802546, 화합물

HRID 2102415노트

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HRID 2102415 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([C:15]([NH:17][NH2:18])=[O:16])=[N:13][N:12]3[CH:19]=[CH:20][N:21]=[C:11]3[CH:10]=2)=[C:4]([F:22])[CH:3]=1.BrC1C=C[C:27]([NH:30]C2C(C(O)=O)=NN3C=CN=C3C=2)=C(F)C=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.NN.CCN(CC)CC>CC(N(C)C)=O.CCOC(C)=O>[NH2:30][C:27]1[O:16][C:15]([C:14]2[C:9]([NH:8][C:5]3[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=3[F:22])=[CH:10][C:11]3[N:12]([CH:19]=[CH:20][N:21]=3)[N:13]=2)=[N:17][N:18]=1

참가 물질

9

반응물 6

HCID 8471TriethylamineHCID 9321HydrazineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 595193857-(4-Bromo-2-fluorophenylamino)-imidazo[1,2-b]pyridazine-6-carboxylic acidHCID 69006850HCID 69006850, 화합물

생성물 1

HCID 57802546HCID 57802546, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 31374Dimethylacetamide용매

실험 절차

Preparation of 7-(4-bromo-2-fluorophenylamino)-imidazo[1,2-b]pyridazine-6-carboxylic acid hydrazide: 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. Hydrazine (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

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

출처 및 근거

ORD 기록
ord-afa3e6fd081d498d9962f0afce73ba1b
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576072B2

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