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1,2-Dichloroethane → 1-benzyl-4-(benzyloxy)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxamide

HRID 1179327
ノート
印刷プレビュー

反応式

HRID 1179327 の反応式
[CH2:1]([N:8]1[C:17]2[C:12](=[N:13][CH:14]=[CH:15][CH:16]=2)[C:11]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:10]([C:26]([OH:28])=O)[C:9]1=[O:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1C=NC2N(O)N=NC=2C=1.C(Cl)CCl.[Cl-].[F:45][C:46]1[CH:51]=[CH:50][C:49]([CH2:52][NH3+:53])=[C:48]([C:54]([NH:56][CH3:57])=[O:55])[CH:47]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:1]([N:8]1[C:17]2[C:12](=[N:13][CH:14]=[CH:15][CH:16]=2)[C:11]([O:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[C:10]([C:26]([NH:53][CH2:52][C:49]2[CH:50]=[CH:51][C:46]([F:45])=[CH:47][C:48]=2[C:54]([NH:56][CH3:57])=[O:55])=[O:28])[C:9]1=[O:29])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-Dichloroethane2 回HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 589780031-Benzyl-4-(benzyloxy)-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxylic acidHCID 866001764-Fluoro-2-[(methylamino)carbonyl]benzylamine hydrochloride

生成物 1

HCID 58977997
1-benzyl-4-(benzyloxy)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-benzyl-4-(benzyloxy)-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxylic acid (0.15 g, 0.39 mmol) in DMF (4 mL) was added HOAT (0.26 g, 1.94 mmol) and EDC (0.07 g, 0.47 mmol). The solution was stirred for 10 minutes at which time EDC (0.036 g, 0.23 mmol), {4-fluoro-2-[(methylamino)carbonyl]phenyl}methanaminium chloride (0.108 g, 0.47 mmol), and DIEA (0.10 g, 0.78 mmol) were added. The reaction was then stirred at room temperature overnight at which time the solution was purified by preparative reverse phase HPLC eluting with a gradient of 5-95% acetonitrile/water (0.1% TFA). The fractions that contained the desired product were concentrated. Note that during the prep des-O-benzyl product was also obtained. The mixture was taken on to the next step.

後処理

  1. additionwere added
  2. customwas purified by preparative reverse phase HPLC
  3. washeluting with a gradient of 5-95% acetonitrile/water (0.1% TFA)
  4. concentrationwere concentrated
  5. customwas also obtained

出典と根拠

ORDレコード
ord-851879903ded4fe497ddd7f4017124e8
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07279487B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート