huagongshe.com
HRID25637

反应详情

EQUATION

反应方程式

HRID 25637 的结构方程式

REACTANTS

反应物

2
结构：C[O-].[Na+]
HCID10942334

Methanol, sodium salt

CH3NaO

结构：CCCN(C)CC#C[C@H]1CC[C@H](N(C)S(=O)(=O)c2ccc(NC(C)=O)cc2)CC1
HCID178457237

未命名化合物

PRODUCTS

生成物

1
结构：CCCN(C)CC#C[C@H]1CC[C@H](N(C)S(=O)(=O)c2ccc(N)cc2)CC1
HCID178457236

未命名化合物

收率 82.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of 44.3 mg (0.1 mmol) of trans-N-[4-(Methyl-{4-[3-(methyl-propyl-amino)-prop-1-ynyl]-cyclohexyl}-sulfamoyl)-phenyl]-acetamide in 5 ml MeOH was treated with 0.37 ml (2 mmol) of sodium methylate (5.4 M in MeOH) and heated at 70° C. for 30 h. The solvent was evaporated and the residue extracted with aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried with Na2SO4, filtered and evaporated. Purification by flash column chromatography on silica gel (CH2Cl2/MeOH 97:3) gave 31 mg (82%) of pure trans-4-Amino-N-methyl-N-{4-[3-(methyl-propyl-amino)-prop-1-ynyl]-cyclohexyl}-benzenesulfonamide, MS: 378 (MH+).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. extractionthe residue extracted with aqueous saturated NaHCO3/Et2O (3×)
  3. dry with materialThe organic phase was dried with Na2SO4
  4. filtrationfiltered
  5. customevaporated
  6. customPurification by flash column chromatography on silica gel (CH2Cl2/MeOH 97:3)