1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10385550、化合物

HRID 1242885ノート

反応式

HRID 1242885 の反応式
CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH2:26].[C:28]1([C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)[CH:33]=[CH:32][C:31]([C:34]([NH:36][C:37]2[CH:45]=[CH:44][C:40]([C:41]([O-])=[O:42])=[CH:39][CH:38]=2)=[O:35])=[CH:30][CH:29]=1>C1COCC1.C(#N)C.C(OCC)(=O)C.O.C(N(CC)CC)C>[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH:26][C:41]([C:40]1[CH:39]=[CH:38][C:37]([NH:36][C:34]([C:31]2[CH:32]=[CH:33][C:28]([C:46]3[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=3)=[CH:29][CH:30]=2)=[O:35])=[CH:45][CH:44]=1)=[O:42]

参加物

10

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 66053N,N-DimethylethylenediamineHCID 757711-HydroxybenzotriazoleHCID 7040114HCID 7040114、化合物

生成物 1

HCID 10385550HCID 10385550、化合物収率 25.3%

試薬・触媒・溶媒 5

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

WSC (0.248 g), HOBt (0.156 g), N,N-dimethyl ethylenediamine (0.097 g) and triethylamine (0.21 ml) were added to a mixed solution of 4-(4-biphenylylcarbonylamino)benzoate (0.323 g) in THF (15 ml) and acetonitrile (15 ml). After stirring at room temperature for 18 hours, water was added to the reaction mixture, and extraction was conducted using ethyl acetate. The organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution, dried, and then concentrated. The residue was recrystallized using methanol/diethyl ether to give the titled compound (0.100 g).

後処理

  1. washThe organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution
  2. customdried
  3. concentrationconcentrated
  4. customThe residue was recrystallized

出典と根拠

ORDレコード
ord-fc5eddb1212c45ee9373ad34bd861204
出典データセット
uspto-grants-2006_10
特許番号
US07115750B1

反応ノート

読み込み中…