Dimethylformamide → HCID 58437409、化合物

HRID 73323ノート

反応式

HRID 73323 の反応式
[CH2:1]([O:8][C:9]([C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][CH:15]=[CH:14]2)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.[OH-].[Na+].CN(C)[CH:29]=[O:30]>>[CH2:1]([O:8][C:9]([C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][CH:15]=[C:14]2[CH:29]=[O:30])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 10264164Benzyl 1H-indole-5-carboxylate

生成物 1

HCID 58437409HCID 58437409、化合物

実験手順

To a solution of 1H-indole-5-carboxylic acid benzyl ester (3.5 g) in N,N-dimethylformamide (30 mL) was added phosphoryl chloride (2.6 g) under ice cooling and this mixture was stirred at room temperature for 2 hours. To this reaction mixture was added 2 mol/L aqueous sodium hydroxide solution until the pH became 6 and this mixture was stirred at 70° C. for 30 minutes. After cooling to ambient temperature, the precipitated solid was collected by filtration, and washed with water and methanol, dried to give the title compound (3.9 g).

後処理

  1. stirringthis mixture was stirred at 70° C. for 30 minutes
  2. temperatureAfter cooling to ambient temperature
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with water and methanol
  5. customdried

出典と根拠

ORDレコード
ord-90bb0dc8680a45d29be8ab15104c07c2
出典データセット
uspto-grants-2014_09
特許番号
US08829040B2

反応ノート

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