Реакция #489705

Уравнение реакции

1-benzyloxy-7-chloro-6-fluoro-isoquinoline

1-Benzyloxy-7-chloro-6-fluoro-isoquinoline

dimethyl acetamide

dioxa-spiro[4.5]decan-8-ol

dimethyl acetamide

sodium hydride

→

crude product

1-Benzyloxy-7-chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-isoquinoline

Условия реакции

Обработка

1. 1
   workup.ADDITIONwas added
2. 2
   Другоеwas continued at room temperature
3. 3
   ДругоеAfter 1 h the solvent was removed under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane
5. 5
   Промывкаwashed with water
6. 6
   СушкаThe organic layer was dried with magnesium sulfate
7. 7
   Другоеevaporated

Методика

1.26 g (8.34 mmol) of dioxa-spiro[4.5]decan-8-ol were dissolved in 50 ml of dimethyl acetamide and 695.2 mg (17.4 mmol) of sodium hydride (60%) were added. After stirring for 30 minutes at room temperature a solution of 2.0 g (6.95 mmol) of 1-benzyloxy-7-chloro-6-fluoro-isoquinoline (11) in 50 ml of dimethyl acetamide was added and stirring was continued at room temperature. After 1 h the solvent was removed under reduced pressure. The residue was dissolved in dichloromethane and washed with water. The organic layer was dried with magnesium sulfate and evaporated, which gave 3.30 g of the crude product, which was used without further purification. Rt=2.05 min (Method C). Detected mass: 426.5 (M+H+).

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