1-Iodoethyl ethyl carbonate synthesis
- Product Name:1-Iodoethyl ethyl carbonate
- CAS Number:80196-04-9
- Molecular formula:C5H9IO3
- Molecular Weight:244.03
50893-36-2
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Yield:80196-04-9 64%
Reaction Conditions:
with sodium iodide in acetonitrile at 60; for 6 h;
Steps:
3
EXAMPLE 3 Synthesis of PGB-02 (3-Aminomethyl-5-methyl-hexanoic acid 1-ethyloxycarbonyloxy-ethyl ester) Procedure: Sodium iodide (3.93 g, 26.2 mmol) was dissolved in anhydrous CH3CN (20 mL). Compound 1 (1.00 g, 6.55 mmol) in anhydrous CH3CN (8 mL) was added and stirred for 6 hours at 60° C. After filtering and concentration, the residue was diluted with ether and re-concentrated to give 1.04 g of Carbonic acid ethyl ester 1-iodo-ethyl ester 2 (Yield: 64%). 1H-NMR (CDCl3, 500 MHz) δ1.32 (t, J=7.0 Hz, 3H), 2.22 (d, J=6.0 Hz, 3H), 4.25 (q, J=7.0 Hz, 2H), 6.75 (q, J=6.0 Hz, 1H); 13C-NMR (CDCl3, 125 MHz) δ 14.14, 30.10, 52.34, 152.48.
References:
US2008/125483,2008,A1 Location in patent:Page/Page column 6
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