Pyridine → HCID 23086661, 화합물

HRID 229733노트

반응식

HRID 229733 반응식
N1C=CC=CC=1.[CH3:7][C:8]1[CH:9]=[C:10]([OH:28])[C:11]2[CH:12]=[C:13]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=3)[N:14]=[N:15][C:16]=2[CH:17]=1.[C:29](OC(=O)C)(=[O:31])[CH3:30]>CCCCCC.C(OCC)(=O)C>[C:29]([O:28][C:10]1[CH:9]=[C:8]([CH3:7])[CH:17]=[C:16]2[C:11]=1[CH:12]=[C:13]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=1)[N:14]=[N:15]2)(=[O:31])[CH3:30]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 1354580247-Methyl-3-(3-trifluoromethylphenyl)cinnolin-5-ol

생성물 1

HCID 23086661HCID 23086661, 화합물수율 36%

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매

실험 절차

To a pyridine solution (2 mL) of 7-methyl-3-(3-trifluoromethylphenyl)cinnolin-5-ol (60 mg, 0.2 mmol) obtained in Example 70 was added acetic anhydride (3 mL), followed by reaction at room temperature over night. The reaction liquid was concentrated under reduced pressure, followed by adding distilled water (1 mL), extraction with ethyl acetate and purification of residue obtained after concentration of an organic layer under reduced pressure, with HPLC column chromatography (hexane/ethyl acetate=3/1) to obtain an objective compound (25 mg, 36%) as pale yellow solid.

후처리

  1. customfollowed by reaction at room temperature over night
  2. customThe reaction liquid
  3. concentrationwas concentrated under reduced pressure
  4. additionby adding
  5. distillationdistilled
  6. extractionwater (1 mL), extraction
  7. customwith ethyl acetate and purification of residue
  8. customobtained after concentration of an organic layer under reduced pressure

출처 및 근거

ORD 기록
ord-243ecda653724554bc1d7723a9b3e920
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563893B2

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