反応 #54989

反応方程式

N,N-dimethyl-2-hydroxyimino-3-methoxyiminobutyramide

methyl isocyanate

triethylenediamine

→

N,N-dimethyl-3-methoxyimino-2-[(methylcarbamoyl)oximino]butyramide

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度refluxed for 1 hour
2. 2
   その他The solvent was removed
3. 3
   その他by stripping under reduced pressure (15 mm.) at 50°
4. 4
   その他affording the solid crude product
5. 5
   その他Recrystallization from a benzene-acetonitrile mixture

実験手順

A mixture of 34 parts of N,N-dimethyl-2-hydroxyimino-3-methoxyiminobutyramide, 350 parts of methylene chloride, 13 parts of methyl isocyanate and one-tenth part triethylenediamine was stirred at 25° C. for 3 hours and then refluxed for 1 hour. The solvent was removed by stripping under reduced pressure (15 mm.) at 50° bath temperature, thereby affording the solid crude product. Recrystallization from a benzene-acetonitrile mixture gave 32 parts of N,N-dimethyl-3-methoxyimino-2-[(methylcarbamoyl)oximino]butyramide, m.p. 172°-173° C.

出典