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Undecanoic acid, 11-[[(1,1-dimethylethoxy)carbonyl]amino]-, 2,5-dioxo-1-pyrrolidinyl ester synthesis

3synthesis methods
-

Yield:176242-02-7 92%

Reaction Conditions:

with 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride in dichloromethane at 20;

Steps:

24 Preparation of intermediate 24f3

Preparation of intermediate 24f3
To a solution of 24f2 (1.2g, 3.98mmol) in DCM (30ml), N-hydroxyl scuccinimide (0.60g, 5.18mmol) was added, followed by EDC (1.0g, 5.18mmol). The solution was stirred at room temperature for overnight. The reaction was conentrated, directly loaded onto Si02 column and purified with 40% ethylacetate/heptane to afford 1.46g compound 24f3 (92% yield). 1 H NMR (CHLOROFORM-d, 400MHz) d: 4.49 (br. s, 1 H), 3.04-3.19 (m, 2H), 2.86 (d, J=4.5 Hz, 4H), 2.62 (t, J=7.4 Hz, 2H), 1.70-1.82 (m, 2H), 1.37-1.53 (m, 13H), 1.30 (br. s., 10H)

References:

WO2015/200078,2015,A1 Location in patent:Page/Page column 225; 226