N,N,N-trimethyl-1,1-bis(1-methylethoxy)amine → 2-Butyl-4-dimethylaminomethylene-2-imidazolin-5-one

A solution of 5.00 g (35.67 mmol) of 2-butyl-2-imidazolin-5-one and 7.02 g (39.24 mmol) of N,N-dimethylformamide diisopropyl acetal in 25 ml of methylene chloride was stirred at room temperature for 2.5 hours. Then, the solvent was removed on a Rotavapor, and the residue was treated with 40 ml of methylene chloride. The solution thus obtained was washed twice, each time with 10 ml of water, and dried (MgSO4) and concentrated on the Rotavapor. The residue was then dried in a high vacuum. 5.37 g of 2-butyl-4-dimethylaminomethylene-2-imidazolin-5-one was obtained; the product had a content of greater than 90 percent, according to H-NMR: This corresponds to a yield of about 71 percent, based on the 2-butyl-2-imidazolin-5-one.

1. customThen, the solvent was removed on a Rotavapor
2. additionthe residue was treated with 40 ml of methylene chloride
3. customThe solution thus obtained
4. washwas washed twice
5. dry with materialeach time with 10 ml of water, and dried (MgSO4)
6. concentrationconcentrated on the Rotavapor
7. customThe residue was then dried in a high vacuum

ORDレコード

ord-df8d1464c1dd4fd1a820dd4c341dc047

出典データセット

uspto-grants-1996_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05536841