反応 #5139

反応方程式

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

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   その他obtained in Reference Example 2
2. 2
   workup.STIRRINGby stirring for further 4 hours
3. 3
   洗浄the mixture was washed with saturated aqueous sodium chloride solution
4. 4
   乾燥After drying over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
6. 6
   その他The obtained crude product
7. 7
   その他was recrystallized from toluene

実験手順

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.

出典