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Trifluoroacetic acid → 4-Methyl-4,6,7,8,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepin-3(2H)-one

HRID 1668568
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HRID 1668568 반응식
[CH3:1][N:2]1[C:7]2=[CH:8][C:9]3[CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11][C:10]=3[CH:23]=[C:6]2[O:5][CH2:4][C:3]1=[O:24].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][N:2]1[C:7]2=[CH:8][C:9]3[CH2:15][CH2:14][NH:13][CH2:12][CH2:11][C:10]=3[CH:23]=[C:6]2[O:5][CH2:4][C:3]1=[O:24]
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 584947921,1-Dimethylethyl 4-methyl-3-oxo-3,4,6,7,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepine-8(2H)-carboxylate

생성물 1

HCID 584946054-Methyl-4,6,7,8,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepin-3(2H)-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1-Dimethylethyl 4-methyl-3-oxo-3,4,6,7,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepine-8(2H)-carboxylate (0.16 g) was treated with TFA (2 ml) in DCM (4 ml) for 3 h at 25° C. After elimination of volatiles under reduced pressure the residue was partitioned between aqueous NaHCO3 and DCM. The organic layer was collected and the aqueous phase extracted twice with DCM. The combined DCM layers were dried (Na2CO3), filtered and concentrated to give the title compound as a colourless solid which was used without further analysis (0.11 g).

후처리

  1. customAfter elimination of volatiles under reduced pressure the residue was partitioned between aqueous NaHCO3 and DCM
  2. customThe organic layer was collected
  3. extractionthe aqueous phase extracted twice with DCM
  4. dry with materialThe combined DCM layers were dried (Na2CO3)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cc0c507d78a34d4486163d449c6b3279
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989444B2

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