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Triethylamine → (S,S)-N-[3-(3-Fluoro-4-{4-[2-(2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6-yloxy)-acetyl]-piperazin-1-yl}-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide

HRID 1446066
ノート
印刷プレビュー

反応式

HRID 1446066 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N:30]2[CH2:34][CH:33]([CH2:35][NH:36][C:37](=[O:39])[CH3:38])[O:32][C:31]2=[O:40])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[CH2:15][O:16][CH:17]2[CH2:22][O:21][C:20]3=[N:23][C:24]([N+:26]([O-:28])=[O:27])=[CH:25][N:19]3[CH2:18]2)[CH2:10][CH2:9]1.[N+](C1N=C2N(C=1)CC(OCC(O)=O)CO2)([O-])=O.FC1C=C(N2CC(CNC(=O)C)OC2=O)C=CC=1N1CCNCC1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(CC)CC>CN(C=O)C.CCOC(C)=O.O>[F:1][C:2]1[CH:3]=[C:4]([N:30]2[CH2:34][C@H:33]([CH2:35][NH:36][C:37](=[O:39])[CH3:38])[O:32][C:31]2=[O:40])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[CH2:15][O:16][C@@H:17]2[CH2:22][O:21][C:20]3=[N:23][C:24]([N+:26]([O-:28])=[O:27])=[CH:25][N:19]3[CH2:18]2)[CH2:10][CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 18939356N-[[3-(3-Fluoro-4-(piperazin-1-YL)phenyl)-2-oxooxazolidin-5-YL]methyl]acetamideHCID 68548045HCID 68548045、化合物HCID 68548178HCID 68548178、化合物

生成物 1

HCID 44242534
(S,S)-N-[3-(3-Fluoro-4-{4-[2-(2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6-yloxy)-acetyl]-piperazin-1-yl}-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide
収率 10%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

N-[3-(3-Fluoro-4-{4-[2-(2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6-yloxy)-acetyl]-piperazin-1-yl}-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide. A mixture of (2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6-yloxy)-acetic acid (53 mg, 0.22 mmol), N-[3-(3-fluoro-4-piperazin-1-yl-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide (73 mg, 0.228 mmol) (prepared as described by Barbachyn et al, U.S. Pat. No. 5,547,950) and TBTU (114 mg, 0.35 mmol) is dissolved in DMF (5 ml) and treated with Et3N (0.122 ml, 0.88 mmol) and stirred at room temperature for 12 hours. The mixture was diluted with EtOAc and water. The organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was purified by preparative TLC to give 13 mg (10%) of the titled product as a tan solid. ESI MS m/z 562 (M+H+); 1H NMR (400 MHz, CDCl3) δ 7.50 (d, J=11.6 Hz, 1H), 7.44 (s, 1H), 7.21-7.02 (m, 1H), 7.00-6.85 (m, 1H), 5.99-5.92 (m, 1H), 4.76-4.67 (m, 2H), 4.44-4.22 (m, 4H), 4.05-4.01 (m, 1H), 3.79-3.44 (m, 4H), 3.49 (s, 2H), 3.10-2.62 (m, 4H), 2.02 (s, 3H), 1.24 (s, 3H).

後処理

  1. customprepared
  2. washThe organic layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by preparative TLC

出典と根拠

ORDレコード
ord-6411674ff451413eb00c5f80d6987ab9
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07666864B2

反応ノート

読み込み中…

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