1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 57665017、化合物

HRID 1717304ノート

反応式

HRID 1717304 の反応式
[CH:1]1([CH2:7][C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([C:19]([NH:21][CH2:22][CH3:23])=[O:20])=[CH:15][CH:14]=3)[N:11]=[N:10][C:9]=2[C:24]([OH:26])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1C=C[C:30]2N(O)N=[N:33][C:31]=2[CH:32]=1.C1(N)CC1.CCN=C=NCCCN(C)C>C(#N)C.CN(C=O)C.C(=O)([O-])O.[Na+].O>[CH:1]1([CH2:7][C:8]2[N:12]([C:13]3[CH:14]=[CH:15][C:16]([C:19]([NH:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH:18]=3)[N:11]=[N:10][C:9]=2[C:24]([NH:33][CH:31]2[CH2:32][CH2:30]2)=[O:26])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

8

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 69828CyclopropylamineHCID 757711-HydroxybenzotriazoleHCID 68513203HCID 68513203、化合物

生成物 1

HCID 57665017HCID 57665017、化合物収率 183.6%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 516892Sodium Bicarbonate溶媒HCID 21891449acetonitrile N,N-dimethylformamide溶媒

実験手順

5-(Cyclohexylmethyl)-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazole-4-carboxylic acid (357 mg, 1.00 mmol) obtained in Example 102b), HOBt (68.2 mg, 0.500 mmol, 0.5 eq.) and cyclopropylamine (0.093 ml, 1.30 mmol, 1.3 eq.) were dissolved in acetonitrile-DMF (2:1, 4.5 ml), WSC (215 mg, 1.10 mmol, 1.1 eq.) was added, and the mixture was stirred at room temperature for 14 hr. Water was added to the reaction mixture, and the obtained suspension was diluted with 2% aqueous sodium hydrogen carbonate solution. The precipitate was collected by filtration, washed with water and dried to give the title compound as a white powder (363 mg, 0.918 mmol, 91.8%).

後処理

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-df5c375ef883454ebe22f0ea1228dee6
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

読み込み中…