Hydrochloric Acid → HCID 86627957, compound

Participants

Reaction Steps

I2 was dissolved in a mixture of THF and H2O (4:1, 0.35M solution) at RT and LiOH.H2O (1.1 eq.) was added and the mixture was then stirred for 1.5 hr. 1M HCl was added until pH 4-5, then the THF was removed under reduced pressure. The aqueous phase was extracted with EtOAc (3×); the collected organic phases were washed with brine and then dried (Na2SO4). After removal of the solvent the title compound was obtained as a colorless oil which solidified upon standing, this was used in the next step without purification. 1H NMR (400 MHz, CDCl3) δ: 5.23 (1H, br. s), 4.13 (1H, br. s), 2.21 (2H, t, J=7.4 Hz), 1.75-1.90 (1H, m), 1.70-1.50 (3H, m), 1.45 (9H, s), 1.44 (9H, s), 1.50-1.25 (4H, m) MS (ES) C17H31NO6 requires: 345, found: 346 (M+H)+.

Provenance & Evidence