Duloxetine IMpurity A synthesis
- Product Name:Duloxetine IMpurity A
- CAS Number:947686-09-1
- Molecular formula:C25H23NO3S
- Molecular Weight:417.52
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Yield:947686-09-1 75.6%
Reaction Conditions:
Stage #1: N-methyl-(S)-duloxetinewith N-ethyl-N,N-diisopropylamine in toluene at 45; for 0.166667 h;
Stage #2: phenyl chloroformate at 55; for 2 h;
Steps:
A mixture of residue 4 obtained above in toluene (250mL) was stirred for 10min. The temperature was increased at 45°C and diisopropylethyl-amine (7.5g) was added with stirring for further 10min. Subsequently, phenyl chloroformate (52.8g, 330mmol) was added dropwise with stirring at 55°C for 2h. Then, the mixture was cooled to 25°C and 1% sodium bicarbonate (150mL) was added and stirred for 10min. The organic layer was successively washed with 0.5N hydrochloric acid solution, 1% sodium bicarbonate and water. The organic phase was concentrated and dissolved in DMSO (300mL) at 45°C followed by adding sodium hydroxide (68g/100g water). The basic mixture was stirred at 55°C for 8h. The obtained mixture was treated as described above, yielding the free base (S)-6
References:
Chen, Xiang;Liu, Zhi-Qiang;Lin, Chao-Ping;Zheng, Yu-Guo [Bioorganic Chemistry,2016,vol. 65,p. 82 - 89]
![(S)-N,N-DIMETHYL-[3-(2-THIENYL)-3-(1-NAPHTHYLOXY)PROPYL]AMINE--PHOSPHORIC ACID (1:1)](/CAS/GIF/161005-84-1.gif)
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