Reaktion #2358260

Reaktionsgleichung

water

methanesulfonyl chloride

5-amino-2,3,4,5-tetrahydro-1-benzoxepine

triethylamine

→

5-methylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine

Ausbeute 74.7%

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto come to RT
2. 2
   workup.DISTILLATIONthe THF was distilled off in vacuo
3. 3
   workup.ADDITIONThe residue was diluted with a further 50 ml of water
4. 4
   workup.STIRRINGstirred for 3 h
5. 5
   Filtrationthe deposited product was filtered off with suction
6. 6
   SonstigeAfter drying in vacuo

Vorschrift

1.54 g (13.4 mmol) of methanesulfonyl chloride were added dropwise with ice cooling to a solution of 2.0 g (12.2 mmol) of 5-amino-2,3,4,5-tetrahydro-1-benzoxepine (Example 6b) and 3.7 g (36.6 mmol) of triethylamine in 40 ml of THF. The mixture was allowed to come to RT and was stirred overnight and treated with 50 ml of water, and the THF was distilled off in vacuo. The residue was diluted with a further 50 ml of water and stirred for 3 h, and the deposited product was filtered off with suction. After drying in vacuo, 2.2 g of 5-methylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine were obtained, m.p. 105-106° C.

Quelle