Phosphorus oxychloride → HCID 17780353、化合物

HRID 2187659ノート

反応式

HRID 2187659 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][C:10]3[C:15]([CH:16]=2)=[CH:14][C:13]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:12][CH:11]=3)=[CH:4][CH:3]=1.C([N:25]1[CH2:29][C:28](=O)[N:27]=[CH:26]1)(=O)C.P(Cl)(Cl)([Cl:33])=O>>[ClH:33].[NH:27]1[CH2:28][CH2:29][N:25]=[C:26]1[C:16]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:17][C:18]([F:21])([F:19])[F:20])[CH:14]=2)[NH:9][C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=1

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 18476298HCID 18476298、化合物HCID 22350258N-acetyl-2-imidazolinone

生成物 1

HCID 17780353HCID 17780353、化合物

反応条件

温度
60 °C

実験手順

380 mg (1.3 mmol) of the indole from Step A was heated with 210 mg (1.6 mmol) of N-acetyl-2-imidazolinone in 1.3 ml of neat phosphoryl chloride at 60° C. for 20 h. The excess of phosphoryl chloride was removed under reduced pressure, and the residue was dissolved in 2 ml of absolute ethanol and heated at 60° C. for 5 h. The mixture was cooled, and the crystalline precipitate collected by filtration, washed with ethanol, and dried in vacuo.

後処理

  1. customThe excess of phosphoryl chloride was removed under reduced pressure
  2. dissolutionthe residue was dissolved in 2 ml of absolute ethanol
  3. temperatureThe mixture was cooled
  4. filtrationthe crystalline precipitate collected by filtration
  5. washwashed with ethanol
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-84807a0a3561482eb676cd05de1762a2
出典データセット
uspto-grants-2002_06
特許番号
US06410562B1

反応ノート

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