Triethylamine → HCID 57802546、化合物

HRID 2102415ノート

反応式

HRID 2102415 の反応式
[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

参加物

9

反応物 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、化合物

生成物 1

HCID 57802546HCID 57802546、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-afa3e6fd081d498d9962f0afce73ba1b
出典データセット
uspto-grants-2009_08
特許番号
US07576072B2

反応ノート

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