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

HRID 1356474ノート

反応式

HRID 1356474 の反応式
[C:1]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]=[CH:5][C:4]([C:7]([NH:9][C:10]2[CH:18]=[CH:17][C:13]([C:14](O)=[O:15])=[CH:12][CH:11]=2)=[O:8])=[CH:3][CH:2]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:46][N:47]([CH3:51])[CH2:48][CH2:49][NH2:50]>C1COCC1.O.C(N(CC)CC)C.C(#N)C>[CH3:46][N:47]([CH3:51])[CH2:48][CH2:49][NH:50][C:14]([C:13]1[CH:12]=[CH:11][C:10]([NH:9][C:7]([C:4]2[CH:5]=[CH:6][C:1]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:2][CH:3]=2)=[O:8])=[CH:18][CH:17]=1)=[O:15]

参加物

9

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 66053N,N-DimethylethylenediamineHCID 757711-HydroxybenzotriazoleHCID 4590482HCID 4590482、化合物

生成物 1

HCID 10385550HCID 10385550、化合物収率 25.4%

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

To a solution of 4-(4-biphenylylcarbonylamino)benzoic acid (0.323 g) in THF (15 ml)/acetonitrile (15 ml) were added WSC (0.248 g), HOBt (0.156 g), N,N-dimethylethylenediamine (0.097 g), and triethylamine (0.21 ml). After stirring at room temperature for 18 hr, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride sequentially, dried, and concentrated. The residue was recrystallized from methanol/diethyl ether to obtain the titled compound (0.100 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride sequentially
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from methanol/diethyl ether

出典と根拠

ORDレコード
ord-f992392759f9421c9254a34c15317e6e
出典データセット
uspto-grants-2003_07
特許番号
US06586475B1

反応ノート

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