huagongshe.com
HRID1256468

反应详情

EQUATION

反应方程式

HRID 1256468 的结构方程式

REACTANTS

反应物

2
结构：CS(=O)(=O)O
HCID6395

Methanesulfonic acid

CH4O3S

结构：COc1cccc2c1nc(C(F)F)n2-c1nc(N2CCOCC2)nc(N2CCN(S(=O)(=O)CCN3CCN(S(C)(=O)=O)CC3)CC2)n1
HCID46917647

未命名化合物

PRODUCTS

生成物

1
结构：COc1cccc2c1nc(C(F)F)n2-c1nc(N2CCOCC2)nc(N2CCN(S(=O)(=O)CCN3CCN(S(C)(=O)=O)CC3)CC2)n1.CS(=O)(=O)O
HCID86645853

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

A suspension of 2-(difluoromethyl)-4-methoxy-1-[4-[4-({2-[4-(methylsulfonyl)-1-piperazinyl]ethyl}sulfonyl)-1-piperazinyl]-6-(4-morpholinyl)-1,3,5-triazin-2-yl]-1H-benzimidazole from the previous step in MeOH (50 mL) was treated with methanesulfonic acid (33 mg, 1.1 equiv.) to give a clear solution. The solvent was removed under vacuum and the residue was washed with EtOAc to give 2-(difluoromethyl)-4-methoxy-1-[4-[4-({2-[4-(methylsulfonyl)-1-piperazinyl]ethyl}sulfonyl)-1-piperazinyl]-6-(4-morpholinyl)-1,3,5-triazin-2-yl]-1H-benzimidazole methanesulfonate: mp (MeOH/EtOAc) 232-235° C.; Anal. Calcd. for C28H42F2N10O9S3.0.5H2O: C, 41.7; H, 5.4; N, 17.4. Found: C, 41.7; H, 5.3; N, 17.2%.

WORKUP

后处理

  1. customto give a clear solution
  2. customThe solvent was removed under vacuum
  3. washthe residue was washed with EtOAc