反応 #1105

ord-8babbf86aa35457596df795b424dbf27

反応方程式

Cl
HCl
[Mg]
magnesium
CCCCCCCCBr
octyl bromide
C1CCOC1
THF
COc1c(NC2CCC(=O)CC2)ccnc1C
4-(4-oxocyclohexylamino)-3-methoxy-2-methylpyridine
C1CCOC1
THF
CCCCC(O)(CCC)N(c1ccnc(C)c1OC)C1CCCCC1
4-[(4-Hydroxy-4-n-octyl)cyclohexylamino]-3-methoxy-2-methylpyridine

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONThe THF is then distilled off in vacuo at room temperature
  2. 2
    抽出the product is extracted from the solution which

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723450uspto-grants-1998_03