成人免费xx,国产又黄又湿又刺激不卡网站,成人性视频app菠萝网站,色天天天天

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

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

Atracurium EP Impurity D synthesis

1synthesis methods
AtracuriuM IMpurity V

1075726-86-1
18 suppliers
inquiry

Atracurium EP Impurity D

1075726-91-8
9 suppliers
inquiry

-

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

Atracurium EP Impurity D Related Search: