反応 #644638

反応方程式

4-{2-amino-5-di-methylamino-benzoylamino}-Nα-(2,6-dichlorobenzoyl)-L-phenylalanine methyl ester

1,1′-carbonyl-diimidazole

→

Nα-(2,6-dichlorobenzoyl)-4-{6-dimethylamino-quinazoline-2,4-[1H,3H]-dion-3-yl}-L-phenylalanine methyl ester

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度the mixture was heated at a temperature
2. 2
   その他After the completion of the reaction
3. 3
   ろ過the resulting crystals were filtered off to thus give 35.6 g of primary crystals
4. 4
   濃縮The filtrate and the wash liquid were concentrated to half
5. 5
   workup.ADDITION200 mL of water was added
6. 6
   その他to thus separate out crystals
7. 7
   ろ過the resulting slurry was filtered
8. 8
   乾燥the resulting crystals were dried to thus give 6.35 g of secondary crystals

実験手順

There was suspended, in 480 mL of acetonitrile, 47.1 g of 4-{2-amino-5-di-methylamino-benzoylamino}-Nα-(2,6-dichlorobenzoyl)-L-phenylalanine methyl ester synthesized in the foregoing step 1, then 15.9 g of 1,1′-carbonyl-diimidazole (CDI) was added to the suspension and then the mixture was heated at a temperature ranging from 55 to 60° C. for 2.5 hours with stirring. After the completion of the reaction, the mixture was cooled to 5° C. and the resulting crystals were filtered off to thus give 35.6 g of primary crystals. The filtrate and the wash liquid were concentrated to half, then 200 mL of water was added thereto to thus separate out crystals, the resulting slurry was filtered and the resulting crystals were dried to thus give 6.35 g of secondary crystals. The physical properties of the resulting compound were found to be in good agreement with those observed for the same compound prepared in the foregoing synthesis Example.

出典