تفاعل #446185

معادلة التفاعل

Compound b

Methyl 11-hydroxy-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

Trifluoroacetic anhydride

2-mercaptoethanol

→

methyl 11-(2-hydroxyethyl)thio-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

المذيبات

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىobtained in Reference Example 2
2. 2
   workup.STIRRINGby stirring for further 4 hours
3. 3
   غسيلthe mixture was washed with saturated aqueous sodium chloride solution
4. 4
   تجفيفAfter drying over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
6. 6
   أخرىThe obtained crude product
7. 7
   أخرىwas recrystallized from toluene

الإجراء التجريبي

In 400 ml of methylene chloride was suspended 40.0 g of Compound b obtained in Reference Example 2. Trifluoroacetic anhydride, 21.0 ml, was added to the suspension followed by stirring at room temperature for an hour. Then, 10.7 ml of 2-mercaptoethanol was added to the mixture followed by stirring for further 4 hours. After 100 ml of methylene chloride was added to the reaction mixture, the mixture was washed with saturated aqueous sodium chloride solution. After drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The obtained crude product was recrystallized from toluene to give 37.6 g of methyl 11-(2-hydroxyethyl)thio-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate as white crystals.

المصدر