6,7-二氟-3,4-二氢异喹啉-1(2H)-酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Using analogous conditions as described in example 1 for the preparation of Compound 1A, 6,7-difluoro-3, 4-dihydroisoquinolin-1(2H)-one (I-49d: 300 mg, 1.6393 mmol) was reacted with 3-iodo-4-methyl-pyridine (359 mg, 1.6393 mmol), 1, 4-dioxane (15 mL), copper iodide (31.2 mg, 0.1639 mmol), trans-N,N′-dimethyl-cyclohexyl-1, 2-diamine (77.3 mL, 0.4917 mmol) and potassium phosphate (868.8 mg, 4.0982 mmol) to afford the crude product. Purification by column chromatography on silica gel (80% ethylacetate in hexane) afforded 110 mg of the product (24% yield). to afford the crude product Purification by column chromatography on silica gel (80% ethylacetate in hexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Using an analogous reaction procedure and workup as described in example 1 for the preparation of intermediate I-1d above, ethyl 3,4-difluorophenethylcarbamate (I-49c: 5 g, 21.8340 mmol) in POCl3 (43.6 mL) was reacted with P2O5 (6.19 g, 43.6681 mmol) at 110° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (50% ethyl acetate in hexane) afforded 800 mg of the product (18.91% yield). an analogous reaction procedure workup as described in example 1 for the preparation of intermediate I-1d above to afford the crude product Purification by column chromatography on silica gel (50% ethyl acetate in hexane)