HCID 57770761, 화합물 → HCID 57770854, 화합물

HRID 2092623노트

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HRID 2092623 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)[CH:8]=[C:9]([NH:11][NH2:12])[CH:10]=1)=[O:4].CN([CH:23]=[N:24][C:25](=O)[CH:26]([CH3:28])[CH3:27])C>CC(O)=O>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)[CH:8]=[C:9]([N:11]2[C:25]([CH:26]([CH3:28])[CH3:27])=[N:24][CH:23]=[N:12]2)[CH:10]=1)=[O:4]

참가 물질

4

반응물 2

HCID 57770761HCID 57770761, 화합물HCID 57770793HCID 57770793, 화합물

생성물 1

HCID 57770854HCID 57770854, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

To a solution of 5-hydrazino-4′-methyl-biphenyl-3-carboxylic acid methyl ester (300 mg, 1.17 mmol) in HOAc (5 mL) was added N-dimethylaminomethylene-isobutyramide (233 mg. 1.4 mmol) in one portion. The mixture was heated to 90° C. for two hours. After removing the excess HOAc, the residue was dissolved in EtOAc and washed with saturated aqueous NaHCO3. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography (ISCO™) to afford 5-(5-isopropyl-[1,2,4]triazol-1-yl)-4′-methyl-biphenyl-3-carboxylic acid methyl ester a yellow solid (293 mg, 74.6%).

후처리

  1. customAfter removing the excess HOAc
  2. dissolutionthe residue was dissolved in EtOAc
  3. washwashed with saturated aqueous NaHCO3
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography (ISCO™)

출처 및 근거

ORD 기록
ord-abefdd1cc0ce4aa28665be7a8e1bda21
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440708B2

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