Acetic Anhydride → HCID 22174840, 화합물

HRID 1796529노트

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HRID 1796529 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:20]=[C:11]3[CH:12]=[CH:13][C:14]([C:16]([F:19])([F:18])[F:17])=[CH:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1.[C:21](OC(=O)C)(=[O:23])[CH3:22].[OH-].[Na+]>S(=O)(=O)(O)O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:20]([C:21](=[O:23])[CH3:22])=[C:11]3[CH:12]=[CH:13][C:14]([C:16]([F:18])([F:17])[F:19])=[CH:15][N:10]3[N:9]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 99217692-(4-FLUOROPHENYL)-6-(TRIFLUOROMETHYL)PYRAZOLO[1,5-A]PYRIDINE

생성물 1

HCID 22174840HCID 22174840, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

To a mixture of 2-(4-fluorophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridine (10.30 g, 36.76 mmol) and acetic anhydride (100 mL) was added conc. sulfuric acid (10 drops) and the mixture was stirred and heated at reflux for 1 hour. The reaction mixture was cooled to room temperature and poured into ice water (300 mL). 2N Aqueous sodium hydroxide solution was added to raise the pH of the solution to about 10 and the resulting orange precipitate was collected by filtration. The solid was washed with water, air-dried, and then dried under vacuum to afford the title compound as an orange solid, 11.87 g (quant.). 1H NMR (DMSO-d6): δ 9.58 (s, 1H), 8.41 (d, 1H, J=9.3 Hz), 7.89 (d, 1H, J=9.5 Hz), 7.74 (m, 2H), 7.39 (m, 2H), 2.22 (s, 3H). MS (ES) 323 (M+1).

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperatureto raise the pH of the solution to about 10
  4. filtrationthe resulting orange precipitate was collected by filtration
  5. washThe solid was washed with water
  6. customair-dried
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-ba0aa6a586a54cd08ce8d1065378a6e0
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030134B2

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