반응 #8445

반응 방정식

DMSO

HBr

N-[3-(3-benzoyl-thioureido)-4-methoxy-phenyl]-acetamide

→

N-(7-acetylamino-4-methoxy-benzothiazol-2-yl)-benzamide

수율 86.0%

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   workup.ADDITIONthe reaction mixture was poured onto 1000 ml
3. 3
   workup.DISTILLATIONdistilled water
4. 4
   workup.STIRRINGthe resulting slurry stirred for 15 min
5. 5
   여과The mixture was then filtered
6. 6
   세척the filter cake washed with water
7. 7
   기타dried in vacuo at 50° C.

실험 절차

To a suspension of 15.0 g (43.7 mmol) N-[3-(3-benzoyl-thioureido)-4-methoxy-phenyl]-acetamide in 200 ml glacial acetic acid was added 7.65 ml (43.6 mmol) of a 5.7 M solution of HBr in acetic acid, and the mixture was heated at 90° C. for 1 h. 2.5 ml (48.0 mmol) DMSO was then added, and stirring continued at 90° C. for 1.5 h. After cooling to room temperature, the reaction mixture was poured onto 1000 ml distilled water, and the resulting slurry stirred for 15 min. The mixture was then filtered, and the filter cake washed with water, then dried in vacuo at 50° C., affording 12.8 g (86%) N-(7-acetylamino-4-methoxy-benzothiazol-2-yl)-benzamide as a light brown solid. ES-MS m/e (%): 342 (M+H+, 100).

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