4,4'-Methylenebis(N,N-dimethylaniline) synthesis
- Product Name:4,4'-Methylenebis(N,N-dimethylaniline)
- CAS Number:101-61-1
- Molecular formula:C17H22N2
- Molecular Weight:254.37
Yield:101-61-1 97.4%
Reaction Conditions:
with NaY Zeolite at 190; for 6 h;Reagent/catalyst;Temperature;
Steps:
2.4. Characterization of MBDMA.
2.4. Characterization of MBDMA. A MBDMA yield of 97%(2.47 g, 0.0097mol) and a MDA conversion of 100% wereattained, when a mixture of MDA (1.98 g, 0.01mol), DMC(27.0 g, 0.30mol), and NaY (1.98 g) was stirred at 190°C for6 h. In this case, the liquid was a mixture consisting ofMBDMA, DMC, and a tiny amount of by-products. Afterdistilling off DMC from the mixture, a light yellow solid wasobtained. The solid was further purified by recrystallizationfrom alcohol, and a crystalline compound was obtainedwhich was identified as MBDMA.Characterization data of MBDMA were listed as follows.4,4-Methylene bis(N,N-dimethylaniline) (MBDMA):IR (KBr) ]/cm-1 3448, 2886, 2804, 1613, 1564, 1521, 1480, 1444,1355, 1342, 1309, 1231, 1189, 1168, 1124, 1071, 949, 829, 795, 568,508; 1H NMR (300MHz, CDCl3) 2.88 (s, 12H, CH3), 3.79(s, 2H, CH2), 6.66-6.68 (m, 4H, Ar-H), 7.03-7.06 (m, 4H,Ar-H); MS, m/z, observed: 255.3 [M]+ + 1, C17H22N2 [M]++ 1 requires: 255.4. For C17H22N2 (254.4); found: 79.94% C,8.63% H, 10.73% N. requires: 80.27% C, 8.72% H, 11.01% N.
References:
Qiu, Zegang;Wang, Kunjie;Li, Zhiqin;Li, Tao;Bai, Jinhao;Yin, Chanjuan;Ye, Xiushen;Liu, Haining [Journal of Chemistry,2018,vol. 2018,art. no. 4627903]
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