Aluminium lithium hydride → HCID 90029703、化合物

HRID 1488181ノート

反応式

HRID 1488181 の反応式
[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

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 90033741HCID 90033741、化合物2 回

生成物 1

HCID 90029703HCID 90029703、化合物収率 89.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5ddd017097634db391df49d07b9850b9
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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