반응 #1878

반응 방정식

N-[trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepin-3-ylmethyl]glycine

formalin

oxalic acid

→

N-[trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepin-3-ylmethyl]-N-methylglycine

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated under reduced pressure
2. 2
   추출the concentrate was subjected to 5 extraction with ethyl acetate
3. 3
   세척The organic layer was washed with an aqueous solution of sodium hydrogencarbonate
4. 4
   기타by drying
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   workup.DISSOLUTIONThe residue was dissolved in 6 ml of methanol
7. 7
   workup.ADDITIONTo the solution were added 0.2 g of potassium carbonate and 2 ml of water
8. 8
   농축The reaction mixture was concentrated under reduced pressure, to which
9. 9
   workup.ADDITIONwas added water
10. 10
    추출followed-by extraction with ether
11. 11
    추출followed by extraction with methylene chloride
12. 12
    세척The organic layer was washed with water
13. 13
    기타dried
14. 14
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

To 0.13 g of ethyl ester of N-[trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepin-3-ylmethyl]glycine obtained in Example 40 were added 2 ml of formalin and 2 ml of oxalic acid: The mixture was heated at 80° C. for 2 hours. The reaction mixture was concentrated under reduced pressure, and the concentrate was subjected to 5 extraction with ethyl acetate. The organic layer was washed with an aqueous solution of sodium hydrogencarbonate, then with water, followed by drying. The solvent was distilled off under reduced pressure. The residue was dissolved in 6 ml of methanol. To the solution were added 0.2 g of potassium carbonate and 2 ml of water. The mixture was stirred for 2 hours at 60° C. The reaction mixture was concentrated under reduced pressure, to which was added water, followed-by extraction with ether. The aqueous layer was acidified to pH 4 with dilute hydrochloric acid, followed by extraction with methylene chloride. The organic layer was washed with water and dried, then the solvent was distilled off under reduced pressure. From the residue was obtained 0.1 g of N-[trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepin-3-ylmethyl]-N-methylglycine as crystals, m.p. 195°-197° C.

출처