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With hydrogenchloride; trichlorophosphate In water at 100 - 120℃; for 6 h;
A mixture of a-2 (0.073 mol) in POC13 (150 ml) was stirred at 100°C. HC1 conc. (around 1.5 ml) was added drop wise very carefully until the dissolution of a-2. The mixture was stirred at 120°C for 6 hours. The solvent was evaporated until dryness. The residue was taken-up in H20/ice, basified with K2CO3 (powder) and extracted with ethylacetate + 10percent methanol. The organic layer was separated, dried (over MgSO4), filtered and the solvent was evaporated until dryness, yielding 13.5 g of intermediate a- 3 (83percent, melting point: 178°C).
83%
With hydrogenchloride; trichlorophosphate In water at 100 - 120℃; for 6 h;
A mixture of a-1 (0.073 mol) in POCl3 (150 ml) was stirred at 100°C. HC1 conc. (around 1.5 ml) was added drop wise very carefully until the dissolution of a-1. The mixture was stirred at 120°C for 6 hours. The solvent was evaporated until dryness. The residue was takenup in H20/ice, basified with K2C03 (powder) and extracted with ethylacetate + 10percent methanol. The organic layer was separated, dried (over MgSO4), filtered and the solvent was evaporated until dryness, yielding 13.5 g of intermediate a-2 (83percent, melting point : 178°C).; A mixture of s-2 (0.073 mol) in POC13 (150 ml) was stirred at 100°C. HC1 cone. (around 1.5 ml) was added drop wise very carefully until the dissolution of s-2. The mixture was stirred at 120°C for 6 hours. The solvent was evaporated until dryness. The residue was taken-up in H2O/ice, basified with K2CO3 (powder) and extracted with ethylacetate + 10percent methanol. The organic layer was separated, dried (over MgSO4), filtered and the solvent was evaporated until dryness, yielding 13.5 g of intermediate s-3 (83percent, melting point: 178°C).
Reference：
[1] Patent: WO2005/58874, 2005, A1, . Location in patent: Page/Page column 39-40
[2] Journal of Medicinal Chemistry, 2008, vol. 51, # 4, p. 875 - 896
[3] Patent: WO2005/58871, 2005, A1, . Location in patent: Page/Page column 40-41; 61-62
LiAlH4 (0. 146 mol) was added portion wise to a solution of tetrahydrofuran (200 ml) at 5C under N2 flow. A solution of b-1 (0.073 mol) in tetrahydrofuran (200 ml) was then added drop wise. The mixture was stirred at 5C for 3 hours. A minimum of H20 was then added, followed by a solution of CH2Cl2/CH30H (90/10). The resulting mixture was dried (over MgSO4), filtered and the solvent was evaporated until dryness, yielding 12.6 g of intermediate b-2 (95%, melting point: 179C).
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