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

HRID 1505228
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HRID 1505228 반응식
[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]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 21226445Aluminium lithium hydride2회HCID 216043632-Isopropoxy-6-methyl-nicotinonitrile

생성물 1

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

시약·촉매·용매 1

HCID 3283
Diethyl Ether
용매
2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85f9c001e53b41529197687bc5573a48
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216975B2

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