反応 #155375

反応方程式

ammonium carbonate

2b

{2-[3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-pyridin-2-yl-amino)-propionylamino]-ethyl}-carbamic acid tert-butyl ester

HCl

→

2-[(4-Carbamimidoyl-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carboxylic acid [2-(2-amino-ethylcarbamoyl)-ethyl]-pyridin-2-yl-amide

溶媒

Ethanol

ethanol

反応条件

後処理

1. 1
   その他evaporated to dryness at 30° C
2. 2
   workup.STIRRINGthe mixture stirred at room temperature over night
3. 3
   その他The solvent was then evaporated
4. 4
   その他the residual material was triturated 5 times with ca. 4 mL of a mixture of dichloromethane/methanol (30:1)
5. 5
   ろ過filtered
6. 6
   その他evaporated in order
7. 7
   その他to separate the product from inorganic salts

実験手順

The product of 2b (1.34 mmol) was added to a saturated HCl solution in dry ethanol (30 mL). The solution was stirred at room temperature for 5 hours, then evaporated to dryness at 30° C. Ethanol (30 mL) and ammonium carbonate (13.0 mmol) were added and the mixture stirred at room temperature over night. The solvent was then evaporated, the residual material was triturated 5 times with ca. 4 mL of a mixture of dichloromethane/methanol (30:1), filtered and evaporated in order to separate the product from inorganic salts.

出典