tert-Butyl methyl ether → (2-Methoxy-4,6-dimethylpyridin-3-yl)methanamine

HRID 577451노트

반응식

HRID 577451 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].CC(OC)(C)C.[CH3:13][O:14][C:15]1[C:20]([C:21]#[N:22])=[C:19]([CH3:23])[CH:18]=[C:17]([CH3:24])[N:16]=1>CC(OC)(C)C.C1COCC1>[CH3:13][O:14][C:15]1[C:20]([CH2:21][NH2:22])=[C:19]([CH3:23])[CH:18]=[C:17]([CH3:24])[N:16]=1

참가 물질

5

반응물 3

HCID 15413tert-Butyl methyl etherHCID 5952762-Methoxy-4,6-dimethylnicotinonitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 28064222(2-Methoxy-4,6-dimethylpyridin-3-yl)methanamine

시약·촉매·용매 1

HCID 22492792Mtbe thf용매

실험 절차

LiAlH4 (48.0 g, 1.27 mol) was added into MTBE (600 mL) portion-wise at room temperature. To the suspension was added 2-methoxy-4,6-dimethylpyridine-3-carbonitrile (Cpd S, 103 g, 0.636 mol) in MTBE/THF (1:1, 600 mL) portion-wise. The reaction mixture was stirred at room temperature for an hour then quenched with water (75 mL). The precipitate was collected by filtration and the solids washed with THF (3×100 mL). The filtrate was concentrated under vacuum to give the 1-(2-methoxy-4,6-dimethylpyridin-3-yl)methanamine (Cpd T), which was used in the next step directly.

후처리

  1. customthen quenched with water (75 mL)
  2. filtrationThe precipitate was collected by filtration
  3. washthe solids washed with THF (3×100 mL)
  4. concentrationThe filtrate was concentrated under vacuum

출처 및 근거

ORD 기록
ord-b59ef436e3ba4dde81607e9951c2a6d6
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040515B2

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