Furfurylamine → HCID 178523028、化合物

HRID 34027

反応式

HRID 34027 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:19]([OH:21])=O)[CH:5]=[C:6]2[C:10]=1[NH:9][N:8]=[C:7]2/[CH:11]=[CH:12]/[C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1.C(N(CC)C(C)C)(C)C.O.ON1C2C=CC=CC=2N=N1.[CH2:42]([NH2:48])[C:43]1[O:47][CH:46]=[CH:45][CH:44]=1.Cl.C(N=C=NCCCN(C)C)C>CN(C)C=O.O.C(OCC)(=O)C>[O:47]1[CH:46]=[CH:45][CH:44]=[C:43]1[CH2:42][NH:48][C:19]([C:4]1[CH:5]=[C:6]2[C:10](=[C:2]([F:1])[CH:3]=1)[NH:9][N:8]=[C:7]2/[CH:11]=[CH:12]/[C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)=[O:21]

参加物

9

反応物 5

HCID 3438FurfurylamineHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 178524526HCID 178524526、化合物

生成物 1

HCID 178523028HCID 178523028、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

376 mg of 7-fluoro-3-[(E)-2-(pyridin-3-yl)-vinyl]-1H-indazole-5-carboxylic acid was dissolved in 10 mL of N,N-dimethylformamide, and added with 903 μl of N,N-diisopropylethylamine, 244 mg of 1-hydroxybenzotriazole monohydrate and 147 μl of furfurylamine, and stirred at room temperature for 10 minutes. The solution was cooled to 0° C., added with 509 mg of 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride, and stirred at room temperature overnight. After diluting with water and ethyl acetate, the organic phase was washed with water and saturated brine, and dried over magnesium sulfate. The solvent was evaporated, and the resultant crude product was purified by silica gel column chromatography, to afford 159 mg of the title compound as yellow crystals.

後処理

  1. temperatureThe solution was cooled to 0° C.
  2. stirringstirred at room temperature overnight
  3. washthe organic phase was washed with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe resultant crude product was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-269af998a4324c23b25959beee1b4acf
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

関連ノート

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