Sodium Hydroxide → HCID 57144728, compound

HRID 345987Notes

Reaction equation

HRID 345987 reaction equation
[CH2:1]([NH:5][C:6]1[N:11]=[C:10]([NH:12][CH2:13][CH2:14][CH2:15][CH3:16])[N:9]=[C:8]([N:17]2[C:22]([CH3:24])([CH3:23])[CH2:21][CH:20]([O:25]C(=O)C3C=CC=CC=3)[CH2:19][C:18]2([CH3:35])[CH3:34])[N:7]=1)[CH2:2][CH2:3][CH3:4].[OH-].[Na+]>CO>[CH2:1]([NH:5][C:6]1[N:11]=[C:10]([NH:12][CH2:13][CH2:14][CH2:15][CH3:16])[N:9]=[C:8]([N:17]2[C:22]([CH3:24])([CH3:23])[CH2:21][CH:20]([OH:25])[CH2:19][C:18]2([CH3:35])[CH3:34])[N:7]=1)[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 56984510HCID 56984510, compound

Product 1

HCID 57144728HCID 57144728, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

10 g of 2,4-bis-butylamino-6-(2,2,6,6-tetramethyl-4-benzoyloxypiperidin-1-yl)1,3,5-triazine (prepared according to Example 8) are heated at reflux for 6 hours with 50 ml of methanol and 50 ml of twenty per cent sodium hydroxide solution. The methanol is distilled off from the reaction mixture in vacuo. 100 ml of toluene and 50 ml of water are added to the residue, shaken thoroughly, the aqueous phase is separated off and the toluene solution is washed three times, each with 50 ml of water. After evaporating the toluene solution, 2,4-bis-butylamino-6-(2,2,6,6-tetramethyl-4-hydroxypiperidin-1yl)-1,3,5-triazine is obtained as a yellowish viscous material. Colorless crystals which melt at 90° C. are obtained by crystallization from acetonitrile.

Workup

  1. distillationThe methanol is distilled off from the reaction mixture in vacuo
  2. addition100 ml of toluene and 50 ml of water are added to the residue
  3. customthe aqueous phase is separated off
  4. washthe toluene solution is washed three times
  5. customAfter evaporating the toluene solution

Sources & evidence

ORD record
ord-838954b763524d1691bee2808eb38601
Source dataset
uspto-grants-1991_10
Patent number
US05059689

Reaction notes

Loading…