反応 #59236

反応方程式

2,4,6-Trichloro-s-triazine

ethylamine hydrochloride

N,N-diisopropylethylamine

→

product 2

収率 68.0%

2-Ethylamino-4,6-Dichloro-s-Triazine

収率 68.0%

反応条件

後処理

1. 1
   workup.STIRRINGThe resultant yellow colored solution was stirred at −5° C. for 1 h
2. 2
   その他the solvents removed under reduced pressure
3. 3
   workup.DISSOLUTIONthe resultant residue was dissolved in 1:1 v/v of ethyl acetate and water
4. 4
   その他The organic layer was separated
5. 5
   洗浄washed with saturated solution of NaHCO3
6. 6
   乾燥dried over Na2SO4
7. 7
   その他The organic solvent was removed under reduced pressure
8. 8
   その他to yield an orange colored solid
9. 9
   その他The solid was triturated with hexane

実験手順

2,4,6-Trichloro-s-triazine (1, 1 g, 5.4 mmol), and ethylamine hydrochloride (0.44 g, 5.4 mmol) were combined in a round bottom flask and cooled to −5° C. using an ice-salt bath. To the cooled, stirred solution was added N,N-diisopropylethylamine (1.88 mL, 10.8 mmol). The resultant yellow colored solution was stirred at −5° C. for 1 h, the solvents removed under reduced pressure, and the resultant residue was dissolved in 1:1 v/v of ethyl acetate and water. The organic layer was separated, washed with saturated solution of NaHCO3, and dried over Na2SO4. The organic solvent was removed under reduced pressure to yield an orange colored solid. The solid was triturated with hexane to yield the product 2 as a yellow-orange powder (0.7 g) with a yield of 68%.

出典