تفاعل #55906

معادلة التفاعل

iodide

4-(-8-chlorodibenz[b,f][1,4]oxazepin-11-yl)-1-methylpyridinium iodide

sodium borohydride

→

8-Chloro-11-(1,2,3,6-tetrahydro-1-methyl-4-pyridyl)-dibenz[b,f][1,4]oxazepine hydrochloride

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling for an additional 30 minutes
2. 2
   أخرىThe reaction is quenched with one ml
3. 3
   workup.ADDITIONof acetone and diluted with 500 ml
4. 4
   غسيلThe ether solution is washed with three 250 ml
5. 5
   تجفيفportions of water, dried with brine
6. 6
   درجة الحرارةThe mixture is cooled
7. 7
   ترشيحfiltered
8. 8
   أخرىgiving a tan solid which
9. 9
   أخرىis crystallized from acetone-ethanol-dimethylformamide yielding the desired product as the hydrochloride, mp. 213°-215° C
10. 10
    أخرىproduces compound as a base mp. 143°-145° C.

الإجراء التجريبي

A 6.23 g. portion of the above iodide salt is suspended in 150 ml. of ethanol and the mixture is cooled in an ice salt bath. A 0.64 g. portion of sodium borohydride is added in portions over 1 minute and the resulting solution is stirred with ice bath cooling for an additional 30 minutes. The reaction is quenched with one ml. of acetone and diluted with 500 ml. of ether. The ether solution is washed with three 250 ml. portions of water, dried with brine and made acidic with hydrochloric acid. The mixture is cooled and filtered giving a tan solid which is crystallized from acetone-ethanol-dimethylformamide yielding the desired product as the hydrochloride, mp. 213°-215° C. Failure to acidify the above ether solution produces compound as a base mp. 143°-145° C.

المصدر