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Triethylamine → [trans-1-Benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-yl]methylamine hydrochloride

HRID 1781
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HRID 1781 반응식
[CH2:1]([N:8]1[C:14]2[CH:15]=[CH:16][C:17]([Cl:19])=[CH:18][C:13]=2[C@@H:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[Cl:26])[O:11][C@H:10]([CH2:27]C(O)=O)[C:9]1=[O:31])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([N:34](CC)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1>CN(C)C=O>[ClH:19].[CH2:1]([N:8]1[C:14]2[CH:15]=[CH:16][C:17]([Cl:19])=[CH:18][C:13]=2[C@@H:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[Cl:26])[O:11][C@H:10]([CH2:27][NH2:34])[C:9]1=[O:31])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 69946821trans-1-Benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

생성물 1

HCID 69947635[trans-1-Benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-yl]methylamine hydrochloride

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

In 5 ml of dimethylformamide was dissolved 1.0 g of trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid obtained obtained in Reference Example 5. To the solution was added 0.3 ml of triethylamine, to which was added dropwise, while stirring under ice-cooling, 0.6 g of diphenylphosphoryl azide. The reaction mixture was stirred for one hour at room temperature, which was then poured into ice-water. The mixture was subjected to extraction with ether. The organic layer was washed with water and dried, which was then concentrated under reduced pressure. The concentrate was dissolved in 100 ml of benzene, which was heated for 30 minutes under reflux. The reaction mixture was concentrated under reduced pressure. To the concentrate was added 6 ml of conc. hydrochloric acid, and the mixture was heated for one hour under reflux. The reaction mixture was concentrated under reduced pressure. The concentrate was made alkaline by the addition of a 5% aqueous solution of potassium carbonate, followed by extraction with ethyl acetate. The organic layer was washed with water and dried, then the solvent was distilled off under reduced pressure. To the residue was added an ethanol solution of 4N hydrochloric acid to lead it to hydrochloride to give 0.85 g of [trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-yl]methylamine hydrochloride as crystals, m.p. 245°-250° C.

후처리

  1. customobtained
  2. customobtained in Reference Example 5
  3. additionto which was added dropwise
  4. temperaturecooling
  5. stirringThe reaction mixture was stirred for one hour at room temperature
  6. extractionThe mixture was subjected to extraction with ether
  7. washThe organic layer was washed with water
  8. customdried
  9. concentrationwhich was then concentrated under reduced pressure
  10. dissolutionThe concentrate was dissolved in 100 ml of benzene
  11. temperaturewhich was heated for 30 minutes
  12. temperatureunder reflux
  13. concentrationThe reaction mixture was concentrated under reduced pressure
  14. additionTo the concentrate was added 6 ml of conc. hydrochloric acid
  15. temperaturethe mixture was heated for one hour
  16. temperatureunder reflux
  17. concentrationThe reaction mixture was concentrated under reduced pressure
  18. additionby the addition of a 5% aqueous solution of potassium carbonate
  19. extractionfollowed by extraction with ethyl acetate
  20. washThe organic layer was washed with water
  21. customdried
  22. distillationthe solvent was distilled off under reduced pressure
  23. additionTo the residue was added an ethanol solution of 4N hydrochloric acid

출처 및 근거

ORD 기록
ord-b53797564a374067960a6e48c29544d3
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05726306

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