반응 #5139

반응 방정식

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

용매

methylene chloride

methylene chloride

반응 조건

후처리

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

실험 절차

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. Them, 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.

출처