The reaction mixture was concentrated, giving a white solid foam (1 mbar) that was dried in vacuo (27.7 g, quant. over two steps) and pulverized.
The remaining mother liquor was concentrated to give the aqueous fraction (280 g).
So, our target was concentrated on giving an appropriate and relevant degradation about (10 30 %) and separating the produced degradation products from the parent drug as possible.
The reaction mixture was filtered through Celite and the filtrate was concentrated to give 40z as a colorless oil.
The reaction mixture was filtered through Celite and the filtrate was concentrated to give 40y as a colorless oil (0.10 g, 90%).
The organic solution was concentrated to give 1.05 g (∼quant). of 11a as an oil.
The resulting solution was filtered, and the filtrate was concentrated to give the enamine, which was used without further purification.
The organic solution was concentrated to give 1.37 g (∼quant). of 11b slightly contaminated with some phtalamide.
The original filtrate was concentrated to give a white slurry that was treated with CHCl3 (200 mL) leading to two layers, which were separated, the lower one being mainly TEA ·HBr.
The extract was concentrated after filtration to give an average yield of 20% w/w.
