海萝胶 → 4-[(4-Hydroxy-4-n-octyl)cyclohexylamino]-3-methoxy-2-methylpyridine

HRID 1009

反应方程式

HRID 1009 反应方程式
[Mg].[CH2:2](Br)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].O=[C:12]1[CH2:17][CH2:16][CH:15]([NH:18][C:19]2[CH:24]=[CH:23][N:22]=[C:21]([CH3:25])[C:20]=2[O:26][CH3:27])[CH2:14][CH2:13]1.Cl.C1C[O:32]CC1>>[OH:32][C:5]([N:18]([CH:15]1[CH2:16][CH2:17][CH2:12][CH2:13][CH2:14]1)[C:19]1[CH:24]=[CH:23][N:22]=[C:21]([CH3:25])[C:20]=1[O:26][CH3:27])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][CH2:3][CH3:2]

参与物

6

反应物 5

HCID 313海萝胶HCID 8028四氢呋喃2 次HCID 81401-溴辛烷HCID 5462224MagnesiumHCID 196939514-(4-Oxocyclohexylamino)-3-methoxy-2-methylpyridine

产物 1

HCID 677539694-[(4-Hydroxy-4-n-octyl)cyclohexylamino]-3-methoxy-2-methylpyridine

实验过程

The Grignard solution is prepared from 0.73 g of magnesium and 6.0 g of octyl bromide in 50 ml of absolute THF. 2.8 g of 4-(4-oxocyclohexylamino)-3-methoxy-2-methylpyridine in 20 ml of THF are added dropwise to the solution. After 2 hours the mixture is acidified with 2N HCl. The THF is then distilled off in vacuo at room temperature and the product is extracted from the solution which is rendered alkaline with methylene chloride. Further working up takes place as in the previous working procedure.

后处理

  1. distillationThe THF is then distilled off in vacuo at room temperature
  2. extractionthe product is extracted from the solution which

来源与证据

ORD记录
ord-8babbf86aa35457596df795b424dbf27
来源数据集
uspto-grants-1998_03
专利号
US05723450

关联笔记

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