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1,8-Diazabicyclo(5.4.0)undec-7-ene → (-)-9-Fluoro-3(S)-methyl-10-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-7-oxo-2,3-dihydro-7H-pyrido-[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid

HRID 1742964
ノート
印刷プレビュー

反応式

HRID 1742964 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 688333Levofloxacin q-acidHCID 190059941-(pyrrolidin-3-yl)-1H-1,2,4-triazole hydrochloride

生成物 1

HCID 53860290(-)-9-Fluoro-3(S)-methyl-10-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-7-oxo-2,3-dihydro-7H-pyrido-[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6bc681907c20481e894d9c29497a675a
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05342846

反応ノート

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