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ChemicalBook CAS DataBase List CN128

CN128 synthesis

3synthesis methods
4(1H)-Pyridinone, 3-hydroxy-1-[(1R)-1-(hydroxymethyl)-2-phenylethyl]-2-methyl-

1335282-04-6
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CN128

1335282-05-7
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Yield:1335282-05-7 63.4%

Reaction Conditions:

with hydrogenchloride in methanol;

Steps:

8 Example 8. (R)-3-Hydroxy-1-(1-hydroxy-3-phenyl propyl-2-)-2-methyl pyridine-4(1H)-one hydrochloride, Number: CN328.

Example 8.
(R)-3-Hydroxy-1-(1-hydroxy-3-phenyl propyl-2-)-2-methyl pyridine-4(1H)-one hydrochloride, Number: CN328.
Treated (R)-3-Hydroxy-1-(1-hydroxy-3-phenyl propyl-2-)-2-methyl pyridine-4(1H)-one (Example 7) with HCl methanol solution to generate hydrochloride.
Then recrystallization resulted in 18.26 g white solid.
The yield was 63.4%. specific rotation [α]18D= +176.26, 1HNMR (DMSO-d6): δ 2.30 (s, 3H), 3.13 (dd, J1=14, J2=5.5, 1H), 3.28 (dd, J1=14, J2=5.5, 1H), 3.87 (m, 2H), 5.08 (m, 1H), 7.20 (m, 5H), 7.48 (m, 1H), 8.62 (m, 1H).

References:

EP2692724,2014,A1 Location in patent:Paragraph 0051; 0052