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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 540468Generated: October 27, 2026

Dimethylformamide → HCID 86682291, compound

https://huagongshe.com/reaction/540468

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDimethylformamideHCID 6228—
ReactantSodium AzideHCID 33557—
ReactantHCID 86682293HCID 86682293—
SolventWaterHCID 962—
SolventEthyl acetate hexaneHCID 21226206—
ProductHCID 86682291HCID 86682291—

Reaction Conditions

Temperature60 °C

Reaction Steps

To a solution of (S)-2-(3-bromo-4-methoxyphenyl)-3-hydroxy-3-methylbutyl 4-methylbenzenesulfonate (58 mg, 0.13 mmol) in 2 mL DMF was added NaN3 (34 mg, 0.52 mmol). The resulting reaction mixture was heated at 60° C. overnight and was then diluted with 10 mL EtOAc/hexane (1:1) and 10 mL water. The layers were separated. The organics were dried over sodium sulfate, filtered and concentrated. Crude product was purified on Combiflash prepacked silica gel column, eluted with hexane to 40% EtOAc in hexane to give 38 mg desired product. 1H NMR (500 MHz, CDCl3): δ 7.49 (d, J=1.9 Hz, 1H), 7.22 (dd, J=2.1, 8.5 Hz, 1H), 6.91 (d, J=8.4 Hz, 1H), 3.93 (s, 3H), 3.9 (m, 1H), 3.71 (m, 1H), 2.82 (m, 1H), 1.28 (s, 3H), 1.17 (s, 3H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08871738B2
Source datasetuspto-grants-2014_10
ORD IDord-b37b15c6bf2f401f9f4b2bbca356c07f
Source noteuspto-grants-2014_10