Ethyl Acetate → HCID 22168453、化合物

HRID 390371

反応式

HRID 390371 の反応式
C[C:2]1(C)[N:7]([O])[C:6](C)(C)[CH2:5][CH:4](O)[CH2:3]1.C1(C(O)=O)CC1.[CH2:19]1[CH2:24][CH2:23][CH:22]([N:25]=[C:26]=[N:27][CH:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)[CH2:21][CH2:20]1.C(OCC)(=O)C>CN(C1C=CN=CC=1)C.ClCCl.CCCCCC>[CH2:31]1[CH2:30][CH2:29][CH:28]([N:27]=[C:26]=[N:25][CH:22]2[CH2:23][CH2:24][CH2:19][CH2:20][CH2:21]2)[CH2:33][CH2:32]1.[CH3:22][N:25]([C:4]1[CH:3]=[CH:2][N:7]=[CH:6][CH:5]=1)[CH3:26]

参加物

8

反応物 4

HCID 8857Ethyl AcetateHCID 10868DicyclohexylcarbodiimideHCID 15655Cyclopropanecarboxylic acidHCID 137994Tempol

生成物 1

HCID 22168453HCID 22168453、化合物

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒HCID 8058Hexane溶媒2 回

実験手順

To a stirred solution of Tempol (1.72 g, 0.01 mmole), cyclopropanecarboxylic acid (0.946 g, 0.011 mmole), and DMAP (0.12, 0.001 mmole) in dichloromethane (25 ml) was added DCC (2.27 g, 0.11 mmole) and the mixture was stirred overnight at room temperature. The mixture was filtered over celite and the solution was evaporated under reduced pressure. The product was isolated by silica gel column chromatography using first hexane and then 10% ethyl acetate in hexane. Yield: 2.26 g (94.1). IR and NMR were consistent with the assigned structure.

後処理

  1. filtrationThe mixture was filtered over celite
  2. customthe solution was evaporated under reduced pressure
  3. customThe product was isolated by silica gel column chromatography

出典と根拠

ORDレコード
ord-63ec673a24ab40a1adfad9ee2f981012
出典データセット
uspto-grants-2013_02
特許番号
US08383648B2

関連ノート

読み込み中…