反応 #481907

反応方程式

7-amino-4-(3-bromoanilino)-quinazoline

crotonic acid chloride

→

desired product

収率 31.2%

But-2-enoic acid [4-(3-bromo-phenylamino)-quinazolin-7-yl]-amide

収率 31.2%

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   workup.ADDITIONWhen the addition
2. 2
   その他the ice bath was removed
3. 3
   ろ過The reaction was filtered
4. 4
   その他to remove the yellow solid which
5. 5
   洗浄was washed with tetrahydrofuran
6. 6
   その他recrystallized from 20 mL of boiling methanol

実験手順

To an ice cold solution of 0.158 g of 7-amino-4-(3-bromoanilino)-quinazoline (J Med Chem, 1985:3482) in 5 mL of tetrahydrofuran was added dropwise a solution of 0.105 g of crotonic acid chloride in 5 mL of tetrahydrofuran. When the addition was complete, the ice bath was removed and the reaction stirred at room temperature for 15 hours. The reaction was filtered to remove the yellow solid which was washed with tetrahydrofuran and recrystallized from 20 mL of boiling methanol to afford 0.060 g of the desired product, mp >250° C.

出典