Discovery of

Reference of 629-09-4, A common heterocyclic compound, 629-09-4, name is 1,6-Diiodohexane, molecular formula is C6H12I2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 42-Amino-4-(6-fluorohexyl)-pentane dioic acid a) (2S.4S)-2-tert-Butoxycarbonylamino-4-(6-iodohexyl)-pentane dioic acid dimethyl ester 5.51 g (20 mmol) of Boc-L-Glutamic acid dimethylester (Advanced Chemtech) were dissolved in 60 mL of tetrahydrofuran (THF) and cooled to -70 0C. 44 mL (44 mmol) of 1 M solution of lithium-bis(trimethylsilyl)amide in THF was added drop wise over a period of 1 hour at -70 0C and stirring was continued over 2 h at -70 0C. Then 20.28 g (60 mmol) of 1,6- diiodohexane were added drop wise and, after 2 h at -70 0C, the cooling bath was removed and 100 mL of 2 N hydrochloric acid and 300 mL of ethyl acetate were added. The organic phase was separated, washed neutral with water, dried over sodium sulphate, filtered and the filtrate was reduced in volume by evaporation. The resulting crude product was chromatographed with hexane / ethyl acetate on silica gel. The resulting fractions were combined and reduced in volume by evaporation. Yield: 0.2 g (2.1 %)MS (ESIpos): m/z = 486 [M+H]+1 H NMR (300 MHz, CHLOROFORM-c/) d ppm 1.20-1.70 (m, 29H) 1.75-2.10 (m, 5H) 2.40- 2.50 (m, 1 H) 3.14-3.20 (m, 2H), 3.50-3.75 (m, 3H), 4.15-4.25 (2H) 4.32-4.42 (m, 1H) 5.00- 5.10 (d, 1H)

The synthetic route of 629-09-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; WO2009/141090; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com