Ethoxyethylamine → N1-Ethyl-5-(2-(((2-ethoxyethyl)amino)carbonyl)amino-4-pyridyl)oxy-1H-1-indolecarboxamide

HRID 2376830ノート

反応式

HRID 2376830 の反応式
[CH2:1]([NH:3][C:4]([N:6]1[C:14]2[C:9](=[CH:10][C:11]([O:15][C:16]3[CH:21]=[CH:20][N:19]=[C:18]([NH:22][C:23](=[O:31])OC4C=CC=CC=4)[CH:17]=3)=[CH:12][CH:13]=2)[CH:8]=[CH:7]1)=[O:5])[CH3:2].[CH2:32]([O:34][CH2:35][CH2:36][NH2:37])[CH3:33]>CN(C)C=O>[CH2:1]([NH:3][C:4]([N:6]1[C:14]2[C:13](=[CH:12][C:11]([O:15][C:16]3[CH:21]=[CH:20][N:19]=[C:18]([NH:22][C:23]([NH:37][CH2:36][CH2:35][O:34][CH2:32][CH3:33])=[O:31])[CH:17]=3)=[CH:10][CH:9]=2)[CH:8]=[CH:7]1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 66970EthoxyethylamineHCID 21949099Phenyl N-(4-(1-(ethylamino)carbonyl-1H-5-indolyl)oxy-2-pyridyl)carbamate

生成物 1

HCID 10454295N1-Ethyl-5-(2-(((2-ethoxyethyl)amino)carbonyl)amino-4-pyridyl)oxy-1H-1-indolecarboxamide収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Phenyl N-(4-(1-(ethylamino)carbonyl-1H-5-indolyl)oxy-2-pyridyl)carbamate (100 mg, 0.24 mmol) was dissolved in N,N-dimethylformamide (1.0 ml), and 2-ethoxyethylamine (0.063 ml, 0.6 mmol) was added while stirred at room temperature. After 1 hour, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and brine, and dried over anhydrous sodium sulfate. After the solvent was distilled off, the crystals were precipitated from ethyl acetate-hexane (1:5), filtered off, and dried under aeration to yield the title compound (100 mg, 0.24 mmol, quantitative) as white crystals.

後処理

  1. customthe reaction mixture was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe crystals were precipitated from ethyl acetate-hexane (1:5)
  6. filtrationfiltered off
  7. customdried under aeration

出典と根拠

ORDレコード
ord-2cb5421565a14391bee86f6e958e0428
出典データセット
uspto-grants-2008_12
特許番号
US07468380B2

反応ノート

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