反応 #56560

反応方程式

ethyl 2-(2-formylaminothiazol-4-yl)acetate

acetic anhydride

ethyl 2-(2-formylimino-2,3-dihydrothiazol-4-yl)acetate

potassium permanganate

→

ethyl 2-(2-formylaminothiazol-4-yl)glyoxylate

溶媒

acetic acid

反応条件

後処理

1. 1
   温度heated at 130° to 135° C.
2. 2
   workup.STIRRINGwith stirring
3. 3
   workup.STIRRINGthe mixture was further stirred for 30 minutes at 130° to 135° C
4. 4
   workup.STIRRINGthe mixture was stirred for 15 hours at 38° to 40° C. under introduction of air at the rate of 6000 ml
5. 5
   その他After the reaction
6. 6
   ろ過the precipitates were collected by filtration
7. 7
   洗浄The precipitates were washed with acetic acid and water in turn
8. 8
   その他dried

実験手順

A mixture of manganous acetate tetrahydrate (120 g.), acetic acid (1000 ml) and acetic anhydride (100 ml.) was stirred for 20 minutes in an oil bath heated at 130° to 135° C., and to the mixture was added potassium permanganate (20 g.) over 5 minutes at 105° to 110° C. with stirring and then the mixture was further stirred for 30 minutes at 130° to 135° C. The mixture was cooled to room temperature, and to the mixture was added ethyl 2-(2-formylaminothiazol-4-yl)acetate, which can be represented as ethyl 2-(2-formylimino-2,3-dihydrothiazol-4-yl)acetate, (53.5 g.), and then the mixture was stirred for 15 hours at 38° to 40° C. under introduction of air at the rate of 6000 ml. per minute. After the reaction, the precipitates were collected by filtration. The precipitates were washed with acetic acid and water in turn and then dried to give ethyl 2-(2-formylaminothiazol-4-yl)glyoxylate, which can be represented as ethyl 2-(2-formylimino-2,3-dihydrothiazol-4-yl)glyoxylate, (41.5 g.), mp 232° to 233° C. (dec.).

出典