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ChemicalBook CAS DataBase List Atracurium EP Impurity D
1075726-91-8

Atracurium EP Impurity D synthesis

1synthesis methods
AtracuriuM IMpurity V

1075726-86-1
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Atracurium EP Impurity D

1075726-91-8
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Yield:1075726-91-8 32%

Reaction Conditions:

in methanol;ethyl acetate at 5 - 25; for 73 h;Purification / work up;Heating / reflux;

Steps:

9B

EXAMPLE 9B[0120] This example describes the preparation of (lR-cis)-l-[(3,4-dimethoxy- phenyl)methyl]-l,2,3,4-tetrahydro-6,7-dimethoxy-2-methyl-2-methoxycarbonylethyl- isoquinolinium iodide by crystallization of isomeric mixture. [0121] A mixture of the cis and the trans isomers of (lR)-l-[(3,4-dimethoxy- phenyl)methyl]-l,2,3,4-tetrahydro-6,7-dimethoxy-2-methyl-2-methoxycarbonylethyl- isoquinolinium iodide (1.0 g), prepared as described in example 9, was admixed with methanol (4 ml) and heated to obtain a solution. Ethyl acetate (6 ml) was added and the solution was cooled to about 25°C and stirred for 1 hour. Subsequently, the mixture was cooled to 5°C and kept at that temperature for 72 hours. The thus formed crystals were collected by filtration, washed with ethyl acetate and dried to afford (lR-cis)-l-[(3,4- dimethoxyphenyl)methyl]-l,2,3,4-tetrahydro-6,7-dimethoxy-2-methyl-2-methoxycarbonyl- ethyl-isoquinolinium iodide, 0.315 g, (32% yield or 45% yield from the cis isomer), HPLC purity 99.6 % with 0.4% of the trans isomer; m.p. 186°-188°C , [α]D -77.9° (c=1.02, CH2Cl2).1R NMR (CDCl3): δ= 2.99 (dd, IH; J=13.8, 9.6 Hz, H11), 3.12 (dd, IH, J= 18.6, 6.6 Hz, H4), 3.22-3.40 (m, 3H, H19 and H4), 3.35 (s, 3H, NCH3), 3.49 (s, 3H, OCH3), 3.64 (dd, IH, J= 13.8, 4.2 Hz, H11), 3.74 (s,3H, COOCH3), 3.73-3.77 (m, IH, H3), 3.80 (s,3H,OCH3), 3.82 (s, 3H, OCH3), 3.85 (s, 3H, OCH3), 4.16 (m, 2H, H18 and H3), 4.38 (m, IH, H18), 5.34 (dd, IH, J= 9.6, 4.2 Hz1H1), 6.10 (s, IH, H8), 6.52 (JJ, IH, J= 8.4, 1.8 Hz, Hn), 6.64 (d, IH, J= 1.8 Hz, H13), 6.66 (s, IH, H5), 6.71 (d, IH, J= 8.4 Hz, H16). 13C NMR (CDCl3): δ= 23.51 (C4), 28.57 (C19), 37.90 (C11), 47.20 (NCH3), 52.83 (COOCH3), 54.14 (C3), 55.82 (OCH3), 55.94 (OCH3), 56.05 (OCH3), 56.62 (OCH3), 58.93 (C18), 70.85 (C1), 110.60 (C5), 111.22 (C16), 112.02 (C8), 113.44 (C13), 120.22 (C10), 121.29 (C9), 122.65 (C17), 126.54 (C12), 147.26 (C6), 148.42 (C14), 149.11 (C15), 149.39 (C7), and 169.96 (C20). ESI+MS (m/z): 444.2 [M+].

References:

WO2008/132746,2008,A1 Location in patent:Page/Page column 28-29

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