Methanol → (3S)-3-Methylpentanamidine hydrochloride

In an argon atmosphere, 1.1 g (20.5 mmol) of ammonium chloride are suspended in 20 ml of toluene and cooled to 0° C. 10.29 ml of a 2M solution of trimethylaluminum in toluene are added dropwise, and the mixture is then stirred at RT for 2 h. 1 g (10.29 mmol) of (3S)-3-methylpentanenitrile is then added. The mixture is then stirred at 80° C. overnight. After cooling to 0° C., 40 ml of methanol are added dropwise, and then the resulting solid is filtered off with suction. It is thoroughly washed with methanol several times, and the combined filtrates are concentrated in vacuo. The residue is suspended in dichloromethane/methanol 10:1 and the insoluble solid is again removed. The filtrate then obtained is concentrated and affords 1.01 g (64% of theory) of the desired product.

1. stirringThe mixture is then stirred at 80° C. overnight
2. temperatureAfter cooling to 0° C.
3. filtrationthe resulting solid is filtered off with suction
4. washIt is thoroughly washed with methanol several times
5. concentrationthe combined filtrates are concentrated in vacuo
6. customthe insoluble solid is again removed
7. customThe filtrate then obtained
8. concentrationis concentrated

ORDレコード

ord-3cfbf8b22e7149d78bf6e429b1bf45a7

出典データセット

uspto-grants-2009_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07488733B2