Dimethylformamide → HCID 58437409、化合物

HRID 1258180ノート

反応式

HRID 1258180 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-382b516fe41a4f54bd2ff47b4e79e6f2
出典データセット
uspto-grants-2013_06
特許番号
US08466152B2

反応ノート

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