Реакция #83111

Уравнение реакции

product

1,4-Dioxa-8-thiaspiro[4,5]decane 8-oxide

acetic anhydride

lutidine

→

desired product

1,4-Dioxa-8-thiaspiro[4,5]decan-7-ol

Растворители

ethyl acetate

Условия реакции

Обработка

1. 1
   Температураis heated at 110°-115° C. for 2.5 hours
2. 2
   Температураheated for 3 hours
3. 3
   Промывкаwashed 2× with 1N hydrochloric acid, water, saturated sodium chloride
4. 4
   Другоеdried
5. 5
   Концентрированиеconcentrated in vacuo
6. 6
   workup.DISSOLUTIONThe residue is dissolved in methylene chloride
7. 7
   Фильтрацияfiltered through a pad of hydrous magnesium silicate

Методика

A mixture of 0.88 g of product from Example 393, 5.0 ml of acetic anhydride and 2.0 ml of lutidine is heated at 110°-115° C. for 2.5 hours, followed by increasing the temperature to 150° C. and then heated for 3 hours. The reaction mixture is diluted with ethyl acetate, washed 2× with 1N hydrochloric acid, water, saturated sodium chloride, dried and concentrated in vacuo. The residue is dissolved in methylene chloride, filtered through a pad of hydrous magnesium silicate and reconcentrated in vacuo to give 0.569 g of the desired product.

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