反応 #54986

反応方程式

N,N-dimethyl-2-hydroxyiminoacetoacetamide

ethanol

methoxyamine hydrochloride

→

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

溶媒

pyridine

反応条件

後処理

1. 1
   温度to warm slowly to 25° C.
2. 2
   温度maintained at this temperature for 18 hours
3. 3
   温度refluxed for one-half hour
4. 4
   その他The solvent was removed under reduced pressure (15 mm.) at 40° C. bath temperature
5. 5
   workup.ADDITIONApproximately 2000 parts of ice water were added
6. 6
   ろ過The solid was filtered
7. 7
   洗浄washed twice with ice water
8. 8
   ろ過filtered
9. 9
   その他dried

実験手順

To a stirred mixture of 336 parts of N,N-dimethyl-2-hydroxyiminoacetoacetamide (a compound of Formula III), 1500 parts ethanol and 203 parts of methoxyamine hydrochloride were added dropwise 210 parts of pyridine over one-half hour while maintaining the reaction mixture at 10° C. by external cooling. The mixture was allowed to warm slowly to 25° C. and maintained at this temperature for 18 hours. Finally, it was stirred and refluxed for one-half hour. The solvent was removed under reduced pressure (15 mm.) at 40° C. bath temperature. Approximately 2000 parts of ice water were added, which caused the residue to solidify. The solid was filtered, washed twice with ice water, filtered, and dried. There was obtained 340 parts of N,N-dimethyl-2-hydroxyimino-3-methoxyiminobutyramide (a compound of Formula II), m.p. 144-147, which is of satisfactory quality for use as an intermediate. The product was, however, recrystallized from ethyl acetate, whereupon it melted at 146°-148°.

出典