With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5061-21-2,2-Bromo-4-butanolide,as a common compound, the synthetic route is as follows.
5061-21-2, General procedure: Anhydrous K2CO3 (5 equiv) was added to the solution of relevantamine (1 equiv) and tetrabutylammonium bromide (TBAB)(0.01 equiv) in the acetonitrile and the mixture was stirred at at0 C for 1.5 h. Then a solution of 3-bromodihydrofuran-2(3H)-one(8) or 3-bromo-5-methyldihydrofuran-2(3H)-one (9) (1 equiv)was added dropwise and stirring was continued for 12-48 h atroom temperature. After the reaction was completed, the precipitatewas filtered off and the filtrate was concentrated under vacuum.Obtained crude products were purified by columnchromatography. Reagents and conditions: 21.25mmol 1 (5.30g), 85mmol K2CO3 (11.75g), 0.65mmol TBAB (0.21g), 21.25mmol 8 (3.50g), 50ml MeCN, 24h; purification by column chromatography (S7); Yield 98%; yellow solid; mp 164.1-165.3C; Rf: 0.89 (S3); 1H NMR (300MHz, chloroform-d) delta ppm 2.30-2.39 (m, 2H(NCHCH2CH2)) 2.41-2.52 (m, 4H(piperidine)) 2.60-2.69 (m, 2H(piperidine)) 2.89 (dt, J=10.64, 5.45Hz, 2H(piperidine)) 3.66 (t, J=9.62Hz, 1H(NCH)) 4.16-4.25 (m, 1H(CH2CH2O)) 4.33-4.40 (m, 1H(CH2CH2O)) 7.09-7.31 (m, 10H(Ar)), ESI-MS (m/z) 334.1 [M+H]+.
The synthetic route of 5061-21-2 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Kowalczyk, Paula; Sa?at, Kinga; Hoefner, Georg C.; Guzior, Natalia; Filipek, Barbara; Wanner, Klaus T.; Kulig, Katarzyna; Bioorganic and Medicinal Chemistry; vol. 21; 17; (2013); p. 5154 – 5167;,
Tetrahydrofuran – Wikipedia
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