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1873-11-6

4-(2-Hydroxyethyl)-4-azatricyclo-[5.2.1.06]dec-8-ene-3,5-dione synthesis

1synthesis methods
85081-16-9 Synthesis
4,7-Methanoisobenzofuran-1,3-dione, 3a,4,7,7a-tetrahydro-, radical ion(1+), (3aα,4β,7β,7aα)- (9CI)

85081-16-9
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Yield:1873-11-6 143.0 g

Reaction Conditions:

in toluene at 30 - 120;

Steps:

39

Nadic anhydride (164.2 g, 1.00 mole) was dissolved in 220 ml of toluene. To the mixture was slowly added ethanolamine (61.1 g, 1.00 mole) at 30-70° C. and then stirred for 7 hours at 100-120° C. to remove water and part of toluene. Afier overnight in room temperature the resulting yellow crystal was filtered and dried to obtain 143.0 g of nadic imide. 1HNMR(DMSO) 1.50(m, 1H), 1.78(m, 1H),3.08(s, 1H), 3.35 (m, 2H), 3.46 (m, 2H), 3.59 (m, 2H), 3.68 (m, 2H), 6.16 (d, 2H).

References:

US2013/317156,2013,A1 Location in patent:Paragraph 0229