Aluminium lithium hydride → HCID 67261360, 화합물

HRID 79309

반응식

HRID 79309 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13](OCC)=[O:14])[CH:10]=[N:9]2)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([CH2:13][OH:14])[CH:10]=[N:9]2)=[CH:18][CH:19]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 44558860ethyl 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxylate

생성물 1

HCID 67261360HCID 67261360, 화합물수율 75.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

To ethyl 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxylate (8.31 g, 31.9 mmol) in THF (100 mL) at 0° C. was added lithium aluminum hydride (1.45 g, 38.3 mmol). The cold bath was removed and the reaction was stirred for 3 hours. The reaction mixture was diluted with Et2O (200 mL) and Celite (10 g) was added to the reaction mixture. The mixture was cooled to 0° C. and sodium sulfate decahydrate was cautiously added to quench the reaction, which was then filtered, and the filter pad was washed with EtOAc (100 mL) and concentrated to provide the desired product (5.26 g).

후처리

  1. customThe cold bath was removed
  2. additionThe reaction mixture was diluted with Et2O (200 mL) and Celite (10 g)
  3. additionwas added to the reaction mixture
  4. additionsodium sulfate decahydrate was cautiously added
  5. customto quench
  6. customthe reaction, which
  7. filtrationwas then filtered
  8. washthe filter pad was washed with EtOAc (100 mL)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a57c2180b57a44a2b6609ca0acbd1b6b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841455B2

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