反应详情

To a solution of 2.03 g (3.788 mmol) of 3-[2(R)-benzyloxypropyl]amino-3-methyl-N-[2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-3(R)-yl]-butanamide trifluoroacetate (Example 10, Step B) in 40 mL of methylene chloride was added 40 mL of water. The mixture was stirred vigorously while sufficient solid potassium carbonate was added to adjust the pH of the aqueous layer to 10-11. Stirring was discontinued and the layers allowed to separate. The organic layer was removed and the aqueous layer extracted twice more with methylene chloride. The combined extracts were dried over potassium carbonate, filtered and solvents removed under vacuum to afford 1.53 g (3.62 mmol, 95%) of the product as a white solid. 1H NMR (400 MHz, DMSO-d6): 1.04 (s, 3H), 1.06 (s, 3H), 1.14 (d, 7 Hz, 3H), 1.90 (m, 1H), 2.21 (m,3H), 2.60 (m,4H), 3.59 (m,1H), 4.23 (m,1H), 4.45 (d,10 Hz,1H),4.53 (d,10 Hz,1H),6.99 (d,8 Hz,1H), 7.12 (t,8 Hz,1H), 7.20-7.35 (m,7H), 8.72 (d,8 Hz,1H), 9.79 (s,1H).

1. additionwas added
2. customto separate
3. customThe organic layer was removed
4. extractionthe aqueous layer extracted twice more with methylene chloride
5. dry with materialThe combined extracts were dried over potassium carbonate
6. filtrationfiltered
7. customsolvents removed under vacuum