Ethyl Acetate → HCID 22168453, 화합물

HRID 390371

반응식

HRID 390371 반응식
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]

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 10868DicyclohexylcarbodiimideHCID 15655Cyclopropanecarboxylic acidHCID 137994Tempol

생성물 1

HCID 22168453HCID 22168453, 화합물

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매HCID 8058Hexane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-63ec673a24ab40a1adfad9ee2f981012
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383648B2

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