diethyl ether

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Synonyms for diethyl ether

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The literature review shows that direct transformation of epoxides to 1,2-diacetates has been obtained in the presence of various catalysts/reagents such as HCl/ZnCl2 [3], BF3 Et2O [4], DBU/LiCl [5], n-Bu4NCl [6], n- Bu4NOAc [7], Bu3P [8], LiClO4 [9], Er(OTf)3 [10], HY zeolite [11], (NH4)3PMo12O40 [12], (TBA)4P- FeW11O39 3H2O [13], ZrO(OTf)2 [14], NaBH4 [15], phosphomolybdic acid or its supported on silica gel [16] and molecular sieves 4A [17].
5.13 g of compound with a yield of 65% and a melting point of 125-122 C was obtained.; Mp: 122-125C (cyclohexane Et2O); 1H-NMR (400 MHz, CDCl3) d 2.12 (s, 3H, - CH3), 3.37 (s, 2H, Pyrazol), 7.12-7.78 (m, 5H Aromatic- H); 13 C NMR (CDCl3) d 24.6, 42.4, 121.6, 121.7, 124.4, 129.00, 129.2, 140.4, 159.5, 172.8; EIMS m/z 174 (M+, 83.36); Anal.
The precipitated complex was filtered off after overnight, washed with hot H2O, cold EtOH and cold Et2O several times and dried in vacuo.
NH4Cl (25 mL), diluted with H2O (75 mL) and partitioned between aqueous and Et2O (3A-100 mL) layers.
Dilution of the reaction mixture with H2O (300 mL), filtration of Pd catalysts over celite-521, extraction with Et2O (4A-300 mL), dryness of organic layer over anhydrous MgSO4 and concentration in vacuo afforded greenish yellow impure oil (37.850 g).
The crude was purified by column chromatography over flash silica (19 cm in height) in a column (6.3 cm diameter) using petrol, 2.5, 5, 7.5, 10, 12.5, 15, 20 and 25% Et2O in petrol (4A-0.8, 1.6, 3A-0.8 and 2.8 L) as eluent to yield 7 as light yellow oil (27.550 g, 60%).
Rf: 0.73 (Et2O), IR (Imax, cm-1): 1700 (C=O, isolated), [(Alpha) ]31 : a"24.1 (c = 1.16, CHCl3);
The resultant white solid was washed three times with Et2O and dried under reduced pressure to get a white solid (1), Yield: 14.33 g (95%), mp 157 AdegC.
General Synthesis of Sulfenamides Amino ester hydrochloride (1.5 mmol) and Et3N (1.1 mg, 1.5 mL) were dissolved in Et2O (15 mL).