Aluminium lithium hydride → N-Methyl-N-[(1-methyl-1H-indazol-3-yl)methyl]amine

HRID 1581679

反应方程式

HRID 1581679 反应方程式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH3:7][NH:8][C:9]([C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:13]([CH3:20])[N:12]=1)=O>C1COCC1>[CH3:20][N:13]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:11]([CH2:9][NH:8][CH3:7])=[N:12]1

参与物

4

反应物 2

HCID 21226445Aluminium lithium hydrideHCID 22593809N,1-dimethyl-1H-indazole-3-carboxamide

产物 1

HCID 7537473N-Methyl-N-[(1-methyl-1H-indazol-3-yl)methyl]amine收率 104%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂2 次

实验过程

A solution of LiAlH4 in THF (1.0 M, 36 mL, 36 mmole) was added slowly to a solution of N,1-dimethyl-1H-indazole-3-carboxamide (3.42 g, 18 mmole) in dry THF (90 mL) at RT. After 2 hr the mixture was heated to a gentle reflux. After 4 hr the mixture was cooled to RT and quenched by dropwise addition of 2.0 M NaOH until a white solid had formed. The mixture was dried (MgSO4) and filtered, and the filtrate was concentrated under reduced pressure to give the title compound (3.28 g, 100%) as an oil: MS (ES) m/e 176 (M+H)+.

后处理

  1. temperatureAfter 2 hr the mixture was heated to a gentle reflux
  2. customquenched by dropwise addition of 2.0 M NaOH until a white solid
  3. customhad formed
  4. dry with materialThe mixture was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure

来源与证据

ORD记录
ord-3ec0c21fa57f43f794380d2e8bc74db5
来源数据集
uspto-grants-2004_05
专利号
US06730684B1

关联笔记

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