4-Aminobiphenyl → N-biphenyl-4-yl-2-Methyl-malonamic acid methyl ester

HRID 1665675

反応式

HRID 1665675 の反応式
C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[C:23]1([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:28]=[CH:27][C:26]([NH2:29])=[CH:25][CH:24]=1.[CH3:36][O:37][C:38](=[O:44])[CH:39]([CH3:43])[C:40](O)=[O:41]>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[CH3:36][O:37][C:38](=[O:44])[CH:39]([CH3:43])[C:40]([NH:29][C:26]1[CH:25]=[CH:24][C:23]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[CH:28][CH:27]=1)=[O:41]

参加物

8

反応物 4

HCID 71024-AminobiphenylHCID 757711-HydroxybenzotriazoleHCID 3006933-Methoxy-2-methyl-3-oxopropanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 57875815N-biphenyl-4-yl-2-Methyl-malonamic acid methyl ester収率 77.7%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

HOBt (245 mg, 1.8 mmol), DMAP (370 mg, 3.0 mmol), EDCI.HCl (348 mg, 1.8 mmol) followed by biphenyl-4-ylamine (307 mg, 1.8 mmol) were added to a stirred solution of 2-methyl-malonic acid monomethyl ester (200 mg, 1.5 mmol) in DMF (3 mL) and the resulting mixture was stirred at ambient temperature overnight. The reaction mixture was then diluted with water and the product was extracted with ethyl acetate. The ethyl acetate layer was washed with brine solution and concentrated under reduced pressure to afford 330 mg (77%) of N-biphenyl-4-yl-2-Methyl-malonamic acid methyl ester.

後処理

  1. extractionthe product was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with brine solution
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-455ba1db926f4928b12bd1c295bb1b98
出典データセット
uspto-grants-2011_10
特許番号
US08039463B2

関連ノート

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