| 89% |
With hydrogen;Raney nickel; In ethanol; water; at 70℃; under 22502.3 Torr; |
Step C: N-[2-(7-Methoxy-1-naphthyl)ethyl]acetamide There are introduced into an 8 litre reactor 136 g of Raney nickel, 2.06 litres of ethanol and 0.23 litre of water. Whilst stirring at 70 C. and under 30 bars of hydrogen, the compound obtained in Step B (0.8 kg), dissolved in acetic anhydride (2.4 litres), is added slowly. At the end of the addition, the reaction mixture is stirred for 1 hour under hydrogen at 30 bars; the reactor is then subjected to decompression and the liquors are filtered. After concentrating the mixture, the residue is crystallized from an ethanol/water 35/65 mixture to yield the title product in a yield of 89% and with a chemical purity of more than 99%. Melting point: 108 C. |
| 89% |
With hydrogen; In ethanol; water; at 70℃; under 22502.3 Torr; |
The reaction was carried out on a larger batch in order to optimise the yield obtained: 136 g of Raney nickel, 2.06 L of ethanol and 0.23 L of water are introduced into an 8 L reactor. Whilst stirring at 70 C. and under 30 bars of hydrogen, the compound obtained in Step D (0.8 kg) dissolved in acetic anhydride (2.4 L) is slowly added. At the end of the addition, the reaction mixture is stirred for 1 hour under hydrogen at 30 bar, the reactor is then decompressed and the liquors are filtered. After concentration of the mixture, the residue is crystallised from a mixture of ethanol/water 35/65 to yield the title product in a yield of 89% and with a chemical purity greater than 99%. Melting point: 108 C. |
| 89% |
With hydrogen; In ethanol; water; at 70℃; under 22502.3 Torr; for 1h; |
136 g of Raney nickel, 2.06 L of ethanol and 0.23 L of water are introduced into an 8-L reactot Whilst stirring at 70 C. and under 30 bars of hydrogen, the compound obtained in Step D above (0.8 kg) dissolved in acetic anhydride (2.4 L) is added slowly. When the addition is complete, the reaction mixture is stirred for 1 hour under hydrogen at 30 bars, and then the reactor is depressurised and the liquors are filtered. Afier concentration of the mixture, the residue is crystallised from a mixture of ethanol/water 35/65 to yield the title product in a yield of 89% and with a chemical purity greater than 99%.10075] Melting point: 108 C. ?H NMR spectroscopic analysis (CD3OD, 300.13MHz, oe in ppm): 8.21 (bs, 1H); 7.74 (d, J=8.9 Hz, 1H); 7.65 (d, J=8.0 Hz, 1H); 7.52 (d, J=2.5 Hz, 1H); 7.31-7.2 (m, 2H); 7.11 (dd, J=8.9 and 2.5 Hz, 1H); 3.96 (s, 3H); 3.52-3.44 (m, 2H); 3.23-3.18 (m, 2H); 1.94 (s, 3H). ?3C NMR spectroscopic analysis (CD3OD, 75.5 MHz, oe in ppm): 173.4 (s); 159.4 (s); 135.1 (s); 134.6 (s); 131.2 (d); 130.8 (s); 128.2 (d); 127.9 (d); 124.2 (d); 119.3 (d); 103.2 (d); 55.9 (q); 41.4 (0; 34.2 (0; 22.6 (q). |
Chemistry
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