반응 #63642

반응 방정식

trans-3,4,4a,5,6,11b-hexahydro-2H-[1]benzoxepino[5,4-b]-1,4-oxazine hydrochloride

triethylamine

chloroacetyl chloride

→

trans-N-chloroacetyl-3,4,4a,5,6,11b-hexahydro-2H-[1]-benzoxepino[5,4-b]-1,4-oxazine

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   세척washed with a dilute solution of hydrochloric acid
2. 2
   세척wash
3. 3
   세척a wash of dilute sodium hydroxide solution
4. 4
   세척finally by a wash of a saturated solution of sodium chloride
5. 5
   건조The reaction mixture is dried over anhydrous magnesium sulfate
6. 6
   기타evaporated to dryness

실험 절차

A solution of 1.21 g of trans-3,4,4a,5,6,11b-hexahydro-2H-[1]benzoxepino[5,4-b]-1,4-oxazine hydrochloride, prepared according to the procedure of Example 2, and 1.65 ml of triethylamine in 25 ml of methylene chloride is treated dropwise with a solution of 0.70 ml of chloroacetyl chloride dissolved in 10 ml of methylene chloride. The reaction mixture is stirred overnight at room temperature, washed with a dilute solution of hydrochloric acid, followed by a water wash, a wash of dilute sodium hydroxide solution and finally by a wash of a saturated solution of sodium chloride. The reaction mixture is dried over anhydrous magnesium sulfate and evaporated to dryness to obtain 1.44 g of trans-N-chloroacetyl-3,4,4a,5,6,11b-hexahydro-2H-[1]-benzoxepino[5,4-b]-1,4-oxazine.

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