Water → 2-Chloro-4-ethylamino-6-(2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine
Reaction equation
[CH2:1]([NH2:3])[CH3:2].[Cl:4][C:5]1[N:10]=[C:9](Cl)[N:8]=[C:7]([N:12]2[C:17]([CH3:19])([CH3:18])[CH2:16][CH2:15][CH2:14][C:13]2([CH3:21])[CH3:20])[N:6]=1.O>C(O)C>[Cl:4][C:5]1[N:10]=[C:9]([NH:3][CH2:1][CH3:2])[N:8]=[C:7]([N:12]2[C:17]([CH3:19])([CH3:18])[CH2:16][CH2:15][CH2:14][C:13]2([CH3:21])[CH3:20])[N:6]=1Participants
5
Procedure
15 g of a 70% aqueous ethylamine solution is added to 28.9 g of 2,4-dichloro-6-(2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (prepared according to Example 1) in 250 ml of ethanol at room temperature. The temperature climbs rapidly to about 35°. The mixture is subsequently stirred at 55° for 12 hours, 25 ml of water are added and the mixture is cooled to 5°. The resulting precipitate is filtered off, washed with 200 ml of water and dried. 2-Chloro-4-ethylamino-6-(2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine is obtained by crystallization from acetonitrile as colorless crystals having a melting point of 148°.
Workup
- customclimbs rapidly to about 35°
- temperaturethe mixture is cooled to 5°
- filtrationThe resulting precipitate is filtered off
- washwashed with 200 ml of water
- customdried
Sources & evidence
- ORD record
- ord-829f34ee84ef4dbf9e59d9d47e2910d8
- Source dataset
- uspto-grants-1991_10
- Patent number
- US05059689
Reaction notes
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