تفاعل #156604

معادلة التفاعل

Triethylamine

trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester

DMF

methanol

→

2-[4-((R)-3-Dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid methyl ester

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe cooled
2. 2
   أخرىreaction mixture
3. 3
   أخرىwas partitioned between water and ethyl acetate
4. 4
   تجفيفThe organic phase was dried over sodium sulfate
5. 5
   تركيزconcentrated
6. 6
   أخرىThe residue was purified by preparative HPLC
7. 7
   أخرىThe product with the molecular weight of 411.48 (C23H26FN3O3) was obtained in this way

الإجراء التجريبي

Triethylamine (1.0 g) and then Pd(dppf)Cl2 (365 mg) were added to a mixture of trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester (2.5 g), DMF (50 mL) and methanol (25 mL). The mixture was heated at 50° C. in an autoclave under a CO atmosphere (5 bar) for 6 hours. The cooled and decompressed reaction mixture was partitioned between water and ethyl acetate. The organic phase was dried over sodium sulfate and concentrated. The residue was purified by preparative HPLC. The product with the molecular weight of 411.48 (C23H26FN3O3) was obtained in this way; MS (ESI): 412 (M+H+).

المصدر