Phenacyl bromide → 6-Phenylimidazo(2,1-b)(1,3,4)thiadiazole
반응식
[NH2:1][C:2]1[S:3][CH:4]=[N:5][N:6]=1.Br[CH2:8][C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=O>C(O)C>[C:11]1([C:9]2[N:1]=[C:2]3[N:6]([CH:8]=2)[N:5]=[CH:4][S:3]3)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1참가 물질
4
실험 절차
10.1 g. of 2-amino-1,3,4-thiadiazole are dissolved in 160 ml. of ethanol, 19.9 g. of α-bromoacetophenone is added and the solution is heated and stirred at reflux for 1 hour. After cooling, the solid is filtered off and dissolved in 750 ml. of water and 40 ml. of 48% hydrobromic acid. This solution is heated at reflux for 1 hour, neutralized by addition of solid ammonium acetate and refluxed 1/2 hour longer. After cooling, the product is collected on a filter, washed with water and dried. The yield of product is 13 g. melting at 127°-130° C. It has the formula: ##STR15##
후처리
- temperaturethe solution is heated
- temperatureat reflux for 1 hour
- temperatureAfter cooling
- filtrationthe solid is filtered off
- dissolutiondissolved in 750 ml
- temperatureThis solution is heated
- temperatureat reflux for 1 hour
- additionneutralized by addition of solid ammonium acetate
- temperaturerefluxed 1/2 hour longer
- temperatureAfter cooling
- customthe product is collected on a filter
- washwashed with water
- customdried
출처 및 근거
- ORD 기록
- ord-1b705e54bd8247948f3e3bde7a458352
- 출처 데이터셋
- uspto-grants-1982_10
- 특허 번호
- US04354970
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