Water → 2,4-Bis-butylamino-6-(2,2,6,6-tetramethyl-4-benzoylpiperidin-1-yl)-1,3,5-triazine
Reaction equation
Cl[C:2]1[N:7]=[C:6](Cl)[N:5]=[C:4]([N:9]2[C:14]([CH3:16])([CH3:15])[CH2:13][CH:12](OC(=O)C3C=CC=CC=3)[CH2:11][C:10]2([CH3:27])[CH3:26])[N:3]=1.[CH2:28]([NH2:32])[CH2:29][CH2:30][CH3:31].[OH-:33].[Na+].O.[C:36]1([CH3:43])[C:37](C)=[CH:38][CH:39]=[CH:40][CH:41]=1>>[CH2:28]([NH:32][C:2]1[N:7]=[C:6]([NH:9][CH2:10][CH2:11][CH2:12][CH3:13])[N:5]=[C:4]([N:9]2[C:10]([CH3:27])([CH3:26])[CH2:11][CH:12]([C:43](=[O:33])[C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[CH2:13][C:14]2([CH3:15])[CH3:16])[N:3]=1)[CH2:29][CH2:30][CH3:31]Participants
Procedure
20.5 g of 2,4-dichloro-6-(2,2,6,6-tetramethyl-4-benzoyloxypiperidin-1-yl)-1,3,5-triazine (prepared according to Example 2) are stirred in 200 ml of xylene with 8.0 g of n-butylamine at reflux for 4 hours. 4.4 g of pulverized sodium hydroxide are added to the reaction mixture and it is stirred for a further 15 hours at reflux. The contents of the flask are cooled to room temperature and, after addition of 100 ml of water, are vigorously stirred until the precipitated salt has completely gone into solution. The aqueous phase is separated off, and the xylene solution is washed three times, each with 100 ml of water, and evaporated in vacuo. The oily residue is dried at 100° and 13 Pa. 2,4-Bis-butylamino-6-(2,2,6,6-tetramethyl-4-benzoylpiperidin-1-yl)-1,3,5-triazine is obtained as a yellowish viscous material.
Workup
- temperatureat reflux for 4 hours
- temperatureat reflux
- stirringare vigorously stirred until the precipitated salt
- customThe aqueous phase is separated off
- washthe xylene solution is washed three times
- customeach with 100 ml of water, and evaporated in vacuo
- customThe oily residue is dried at 100°
Sources & evidence
- ORD record
- ord-6ec7564c092242d599acd3e691bce00e
- Source dataset
- uspto-grants-1991_10
- Patent number
- US05059689
Reaction notes
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