تفاعل #531334

معادلة التفاعل

11-chloro ester

Methyl 11-Chlorodibenzo[b,f][1,4]thiazepin-3-carboxylate 5,5-Dioxide

morpholine

→

title product

Methyl 11-Morpholinodibenzo[b,f][1,4]thiazepin-3-carboxylate 5,5-Dioxide

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةReflux
2. 2
   workup.DISTILLATIONDistill off the acetonitrile under a vacuum
3. 3
   workup.DISSOLUTIONdissolve the residue in 45 ml of methanol at room temperature
4. 4
   ترشيحFilter
5. 5
   درجة الحرارةcool
6. 6
   أخرىseparate the precipitate
7. 7
   ترشيحby filtration
8. 8
   أخرىRecrystallize from ethanol

الإجراء التجريبي

Reflux a mixture of 5.025 mg (15 mmole) of the 11-chloro ester of Example 14. 3.119 gm of morpholine and 75 ml of acetonitrile for 2 hours. Distill off the acetonitrile under a vacuum and dissolve the residue in 45 ml of methanol at room temperature. Filter, cool and separate the precipitate by filtration. Chromatograph over silica gel eluting with 1:4 ethylacetate in toluene. Recrystallize from ethanol to obtain the title product (m.p. 164°-166° C.).

المصدر