Aluminium lithium hydride → HCID 90029703, 화합물

HRID 1488181노트

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HRID 1488181 반응식
[CH2:1]([N:8]1[CH:12]=[C:11]([CH3:13])[C:10]([C:14](OCC)=[O:15])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH2:1]([N:8]1[CH:12]=[C:11]([CH3:13])[C:10]([CH2:14][OH:15])=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 90033741HCID 90033741, 화합물2회

생성물 1

HCID 90029703HCID 90029703, 화합물수율 89.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Into a 100-mL 3-neck round-bottom flask, which was purged and maintained with an inert atmosphere of nitrogen, was placed a solution of ethyl 1-benzyl-4-methyl-1H-pyrazole-3-carboxylate (compound 268.1, 2.3 g, 9.42 mmol) in THF (30 mL). The solution was cooled to 0° C., then LiAlH4 (360 mg, 9.49 mmol, 1.00 equiv) was carefully added in portions. The resulting mixture was stirred for 1 h at room temperature, then carefully quenched by drop-wise addition of water (400 μL), then aqueous NaOH (10%, 400 μL), followed by additional water (1.2 mL). The solids were removed by filtration and the filtrate was dried (Na2SO4), filtered and concentrated under reduced pressure to obtain the tile compound as a yellow oil (1.7 g, 89%).

후처리

  1. customInto a 100-mL 3-neck round-bottom flask, which was purged
  2. temperaturemaintained with an inert atmosphere of nitrogen
  3. customcarefully quenched by drop-wise addition of water (400 μL)
  4. customThe solids were removed by filtration
  5. dry with materialthe filtrate was dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5ddd017097634db391df49d07b9850b9
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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