Extracurricular laboratory: Synthetic route of 5096-11-7

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5096-11-7, (S)-1-(3-Pyridyl)ethanol, and friends who are interested can also refer to it.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.5096-11-7, name is (S)-1-(3-Pyridyl)ethanol, molecular formula is C7H9NO, molecular weight is 123.15, as common compound, the synthetic route is as follows.Computed Properties of C7H9NO

EXAMPLE 6 (+)-(R)-1-(3-Pyridyl)ethyl 1-adamantanecarboxylate The method followed that described in Example 1, but using (+)-(R)-1-(3-pyridyl)ethanol [87% ee; prepared by asymmetric reduction of 3-acetylpyridine with (+)-B-chlorodiisopinocampheyl borane, J. Chandrasekharan, P. V. Ranachandran and H. C. Brown, J. Org. Chem., 50, 5446-5448 (1985)] (0.62 g, 5.0 mmol) in THF (20 ml), n-butyllithium (2.5 M; 2.0 ml, 5.0 mmol) in hexane, and 1-adamantanecarbonyl chloride (1.09 g, 5.5 mmol) in THF (5 ml). Chromatography, on elution with ether-petrol-triethylamine 100:50:1, gave the title compound (1.16 g, 81%) as an oil. [alpha]D +29.9 (c 2, MeOH), 87% ee. Recrystallisation of the (-)-(1R)-10-camphorsulfonate salt from ethyl acetate, and reliberation of the free-base, afforded the title compound with 98% ee, [alpha]D +33.7 (c 2, MeOH). IR numax 1728 cm-1; 1 H-NMR (CDCl3) delta1.54 (3H, d, J 6.5 Hz, CHCH3), 1.72 and 1.90 (12H, 2s, adamantyl CH2), 2.03 (3H, s, adamantyl CH), 5.88 (1H, q, J 6.5 Hz, CHCH3), 7.30 (1H, m, Py 5-H), 7.65 (1H, m, Py 4-H), 8.56 (1H, m, Py 6-H), 8.63 (1H, m, Py 2-H); MS m/z 285 (M+). Anal. Calcd: C, 75.76; H, 8.12; N, 4.91. Found: C, 75.30; H, 8.18; N, 4.46%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5096-11-7, (S)-1-(3-Pyridyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; British Technology Group Limited; US5595995; (1997); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Extracurricular laboratory: Synthetic route of 5096-11-7

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5096-11-7, (S)-1-(3-Pyridyl)ethanol, and friends who are interested can also refer to it.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.5096-11-7, name is (S)-1-(3-Pyridyl)ethanol, molecular formula is C7H9NO, molecular weight is 123.15, as common compound, the synthetic route is as follows.Computed Properties of C7H9NO

EXAMPLE 6 (+)-(R)-1-(3-Pyridyl)ethyl 1-adamantanecarboxylate The method followed that described in Example 1, but using (+)-(R)-1-(3-pyridyl)ethanol [87% ee; prepared by asymmetric reduction of 3-acetylpyridine with (+)-B-chlorodiisopinocampheyl borane, J. Chandrasekharan, P. V. Ranachandran and H. C. Brown, J. Org. Chem., 50, 5446-5448 (1985)] (0.62 g, 5.0 mmol) in THF (20 ml), n-butyllithium (2.5 M; 2.0 ml, 5.0 mmol) in hexane, and 1-adamantanecarbonyl chloride (1.09 g, 5.5 mmol) in THF (5 ml). Chromatography, on elution with ether-petrol-triethylamine 100:50:1, gave the title compound (1.16 g, 81%) as an oil. [alpha]D +29.9 (c 2, MeOH), 87% ee. Recrystallisation of the (-)-(1R)-10-camphorsulfonate salt from ethyl acetate, and reliberation of the free-base, afforded the title compound with 98% ee, [alpha]D +33.7 (c 2, MeOH). IR numax 1728 cm-1; 1 H-NMR (CDCl3) delta1.54 (3H, d, J 6.5 Hz, CHCH3), 1.72 and 1.90 (12H, 2s, adamantyl CH2), 2.03 (3H, s, adamantyl CH), 5.88 (1H, q, J 6.5 Hz, CHCH3), 7.30 (1H, m, Py 5-H), 7.65 (1H, m, Py 4-H), 8.56 (1H, m, Py 6-H), 8.63 (1H, m, Py 2-H); MS m/z 285 (M+). Anal. Calcd: C, 75.76; H, 8.12; N, 4.91. Found: C, 75.30; H, 8.18; N, 4.46%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5096-11-7, (S)-1-(3-Pyridyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; British Technology Group Limited; US5595995; (1997); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem