반응 #54989

반응 방정식

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

methyl isocyanate

triethylenediamine

→

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

용매

methylene chloride

반응 조건

후처리

1. 1
   온도refluxed for 1 hour
2. 2
   기타The solvent was removed
3. 3
   기타by stripping under reduced pressure (15 mm.) at 50°
4. 4
   기타affording the solid crude product
5. 5
   기타Recrystallization from a benzene-acetonitrile mixture

실험 절차

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.

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