Phosphorus oxychloride → HCID 17780353, 화합물

HRID 2187659노트

반응식

HRID 2187659 반응식
[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

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 18476298HCID 18476298, 화합물HCID 22350258N-acetyl-2-imidazolinone

생성물 1

HCID 17780353HCID 17780353, 화합물

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-84807a0a3561482eb676cd05de1762a2
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06410562B1

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