反応 #357887

反応方程式

4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde

(3-amino-2,6-dichloro-phenyl)-acetonitrile

K2CO3

→

title intermediate

収率 80.0%

6-(3-Amino-2,6-dichloro-phenyl)-2-methylsulfanyl-pyrido[2,3-d]pyrimidin-7-ylamine

収率 80.0%

溶媒

DMF

反応条件

後処理

1. 1
   温度The solution is cooled to room temperature
2. 2
   その他the solid is removed
3. 3
   ろ過by filter paper
4. 4
   濃縮concentrated
5. 5
   その他to give crude product
6. 6
   その他Flash silica gel column purification
7. 7
   洗浄eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%)

実験手順

A mixture of 4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (2.0 g, 11.82 mmol), (3-amino-2,6-dichloro-phenyl)-acetonitrile (2.85 g, 14.18 mmol) and K2CO3 (4.9 g, 35.49 mmol) in DMF (20 mL) is heated to 110° C. for 30 hours. The solution is cooled to room temperature and the solid is removed by filter paper and concentrated to give crude product. Flash silica gel column purification, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%), gives the title intermediate as a solid (3.31 g, 80.0%).

出典