1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 86748098, 화합물

HRID 1742984

반응식

HRID 1742984 반응식
Cl.[N:2]1([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][N:4]=[N:3]1.C1CCN2C(=NCCC2)CC1.[F:24][C:25]1[C:26](F)=[C:27]2[O:32][CH2:31][C@H:30]([CH3:33])[N:29]3[CH:34]=[C:35]([C:40]([OH:42])=[O:41])[C:36](=[O:39])[C:37]([CH:38]=1)=[C:28]23>C(#N)C>[F:24][C:25]1[C:26]([N:10]2[CH2:11][CH2:12][CH:7]([N:2]3[CH:6]=[CH:5][N:4]=[N:3]3)[CH2:8][CH2:9]2)=[C:27]2[O:32][CH2:31][C@H:30]([CH3:33])[N:29]3[CH:34]=[C:35]([C:40]([OH:42])=[O:41])[C:36](=[O:39])[C:37]([CH:38]=1)=[C:28]23

참가 물질

5

반응물 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 688333Levofloxacin q-acidHCID 190060184-(1H-1,2,3-triazol-1-yl)piperidine hydrochloride

생성물 1

HCID 86748098HCID 86748098, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-(1,2,3-triazol-1-yl)piperidine hydrochloride (100 mg) and DBU (80 mg) were added to a suspension of (-)-9,10-difluoro-3(S)-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de]-1,4-benzoxazine-6-carboxylic acid in acetonitrile (5 ml). The reaction mixture was refluxed for 48 hrs followed by stirring at room temperature for an additional 48 hrs. The reaction mixture was concentrated and the residue was diluted with water. The separated solid was filtered, washed with water and dried to yield 30 mg of desired product. m.p. 254°-255° C. (dec). 1H NMR (TFA) δ: 9.4 (s, 1H), 8.67 (s, 1H), 8.57 (s, 1H), 8.16 (d, 11.43Hz, 1H), 5.6-5.1 (m, 2H), 5.0-4.7 (m, 2H), 4.45-4.05 (m, 4H), 3.1-2.6 (m, 4H), 1.86 (d, 6.3Hz, 3H). Anal. calcd. for C 20 H20FN5O4 . H2O; C, 55.68; H, 5.14; N, 16.23.Found C, 55.88; H, 4.762; N, 15.92.

후처리

  1. temperatureThe reaction mixture was refluxed for 48 hrs
  2. concentrationThe reaction mixture was concentrated
  3. additionthe residue was diluted with water
  4. filtrationThe separated solid was filtered
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-45cff9e0cb794ad08d8deb25bc396a95
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05342846

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