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Water → [2-Isopropoxy-6-methyl-3-pyridyl]methanamine

HRID 1505228
ノート
印刷プレビュー

反応式

HRID 1505228 の反応式
[CH:1]([O:4][C:5]1[C:10]([C:11]#[N:12])=[CH:9][CH:8]=[C:7]([CH3:13])[N:6]=1)([CH3:3])[CH3:2].C1COCC1.[H-].[H-].[H-].[H-].[Li+].[Al+3].O>CCOCC>[CH:1]([O:4][C:5]1[C:10]([CH2:11][NH2:12])=[CH:9][CH:8]=[C:7]([CH3:13])[N:6]=1)([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 21226445Aluminium lithium hydride2 回HCID 216043632-Isopropoxy-6-methyl-nicotinonitrile

生成物 1

HCID 61655597[2-Isopropoxy-6-methyl-3-pyridyl]methanamine収率 89.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
溶媒
2 回

反応条件

温度
0 °C

実験手順

The nitrile 32a (1.25 g, 7.12 mmol) solubilized in Et2O (20 mL) and THF (10 mL) was added in small portion to a mixture of LiAlH4 (0.54 g, 2 mol eq) in Et2O (50 mL) stirred at 0° C. Then the mixture was stirred at room temperature overnight. The excess of LiAlH4 was decomposed by water addition at 0° C., the solid formed was filtered, washed with Et2O and the filtrate was separated. The organic phase was anhydrified over Na2SO4 and evaporated to dryness to obtain 33a as yellow oil (1.14 g, 6.35 mmol, 89% Yield) used without further purification.

後処理

  1. stirringThen the mixture was stirred at room temperature overnight
  2. customthe solid formed
  3. filtrationwas filtered
  4. washwashed with Et2O
  5. customthe filtrate was separated
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-85f9c001e53b41529197687bc5573a48
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216975B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート