1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 53860290, 화합물

HRID 1742964

반응식

HRID 1742964 반응식
[F:1][C:2]1[C:3](F)=[C:4]2[O:9][CH2:8][C@H:7]([CH3:10])[N:6]3[CH:11]=[C:12]([C:17]([OH:19])=[O:18])[C:13](=[O:16])[C:14]([CH:15]=1)=[C:5]23.Cl.[N:22]1([CH:27]2[CH2:31][CH2:30][NH:29][CH2:28]2)[CH:26]=[N:25][CH:24]=[N:23]1.C1CCN2C(=NCCC2)CC1>C(#N)C>[F:1][C:2]1[C:3]([N:29]2[CH2:30][CH2:31][CH:27]([N:22]3[CH:26]=[N:25][CH:24]=[N:23]3)[CH2:28]2)=[C:4]2[O:9][CH2:8][C@H:7]([CH3:10])[N:6]3[CH:11]=[C:12]([C:17]([OH:19])=[O:18])[C:13](=[O:16])[C:14]([CH:15]=1)=[C:5]23

참가 물질

5

반응물 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 688333Levofloxacin q-acidHCID 19005994HCID 19005994, 화합물

생성물 1

HCID 53860290HCID 53860290, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 70.25 mg (0.25 mmol) of (-) -9,10-difluoro-3(S)-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de]-1,4-benzoxazine-6-carboxylic acid and 87 mg (0.5 mmol) of 3-(1,2,4-triazol-1-yl)pyrrolidine hydrochloride in 3 ml of acetonitrile in the presence of 76 mg (0.5 mmol) DBU was stirred under nitrogen at reflux condition overnight. The yellow solution was then evaporated to dryness and to the residue, water was added and solid collected. The off-white solid was dissolved in chloroform and the small amounts of the suspension were filtered off. The supernatant was evaporated and to the residue, water was added and solid collected (60 mg), m.p. 229°-231° C. 1H NMR (CDCl3) δ: 8.59 (s, 1H), 8.26 (s, 1H), 7.98 (s, 1H), 7.7 (d, 13.5Hz, 1H), 5.17-5.00 (m, 1H), 4.6-3.73 (m, 7H), 2.67-2.4 (m, 2H), 1.61 (d, 6.7Hz, 3H).

후처리

  1. temperatureat reflux condition overnight
  2. customThe yellow solution was then evaporated to dryness and to the residue, water
  3. additionwas added
  4. customsolid collected
  5. dissolutionThe off-white solid was dissolved in chloroform
  6. filtrationthe small amounts of the suspension were filtered off
  7. customThe supernatant was evaporated and to the residue, water
  8. additionwas added
  9. customsolid collected (60 mg), m.p. 229°-231° C

출처 및 근거

ORD 기록
ord-6bc681907c20481e894d9c29497a675a
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05342846

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