Diisopropylamine → N,N,N',N'-tetraisopropylformamidinium chloride

温度

0 °C

A mixture of phosphorus oxychloride (10.58 g) and diethyl ether (50 ml) is stirred at 0° C. for 10 min. Diisopropylformamide (8.91 g) in diethyl ether (20 ml) is then added drop-wise over a period of 10 min. The resulting mixture is then stirred at room temperature for 30 min. The formed precipitate is allowed to settle and the supernatant removed. Dichloromethane (60 mL) is then added to the mixture. Diisopropylamine (6.98 g) in dichloromethane (20 ml) is then added drop-wise at 0° C. over 10 min. The mixture is then warmed at room temperature and stirred for a further 1.5 h. Diethyl ether (30 ml) is added and the resulting precipitate is removed by filtration. The mother liquor is concentrated in vacuo. Acetone (30 ml) is added and the mixture filtered. The mother liquor is then concentrated in vacuo and subsequently is crystallised with diethyl ether (30 ml) to give N,N,N′,N′-tetraisopropylformamidinium chloride (18, R6=iPr, R7=iPr). 1H NMR (DMSO-d6), 7.49 (1H), 4.15-3.95 (4H), 1.33 (12H), 1.31 (12H).

1. stirringThe resulting mixture is then stirred at room temperature for 30 min
2. temperatureThe mixture is then warmed at room temperature
3. stirringstirred for a further 1.5 h
4. customthe resulting precipitate is removed by filtration
5. concentrationThe mother liquor is concentrated in vacuo
6. additionAcetone (30 ml) is added
7. filtrationthe mixture filtered
8. concentrationThe mother liquor is then concentrated in vacuo
9. customsubsequently is crystallised with diethyl ether (30 ml)

ORDレコード

ord-b3d399308a7b4c489319be48bc3ceea4

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09227934B2