反应详情

To 800 mg (2.88 mmol) 7-(2-hydroxy-ethyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (preparation 7c) in 10 mL DCM is added at 0° C. subsequently 0.34 mL (4.33 mmol) pyridine and 605 mg (3.17 mmol) 4-methyl-benzenesulfonyl chloride in 5.0 mL DCM. The reaction mixture is warmed to RT and is stirred 5 h at RT. Additional 0.34 mL (4.33 mmol) pyridine and 605 mg (3.17 mmol) 4-methyl-benzenesulfonyl chloride in 5.0 mL DCM are added and the mixture is stirred over night. The reaction mixture is poured into ice-water and the organic phase is separated, washed with aqueous KHSO4-solution and aqueous NaHCO3-solution, dried over MgSO4. After evaporation of the solvent, the residue is purified via chromatography (silica gel; cyclohexane/EtOAc 8:2 to 1:1).

1. stirringthe mixture is stirred over night
2. customthe organic phase is separated
3. washwashed with aqueous KHSO4-solution and aqueous NaHCO3-solution
4. dry with materialdried over MgSO4
5. customAfter evaporation of the solvent
6. customthe residue is purified via chromatography (silica gel; cyclohexane/EtOAc 8:2 to 1:1)