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

HRID 2215508ノート

反応式

HRID 2215508 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-37a4786540554f72a277addd115d9462
出典データセット
uspto-grants-2006_09
特許番号
US07109219B2

反応ノート

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