Ethyl Acetate → 627085-11-4

HRID 1169696

반응식

HRID 1169696 반응식
[CH3:1][C:2]1([CH3:12])[N:7]([O])[C:6]([CH3:10])([CH3:9])[CH2:5][CH:4]([OH:11])[CH2:3]1.[CH:13]1([C:16](O)=[O:17])[CH2:15][CH2:14]1.C1CCC(N=C=NC2CCCCC2)CC1.C(OCC)(=[O:36])C>CN(C1C=CN=CC=1)C.ClCCl.CCCCCC>[OH:36][N:7]1[C:2]([CH3:12])([CH3:1])[CH2:3][CH:4]([O:11][C:16]([CH:13]2[CH2:15][CH2:14]2)=[O:17])[CH2:5][C:6]1([CH3:10])[CH3:9]

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 10868DicyclohexylcarbodiimideHCID 15655Cyclopropanecarboxylic acidHCID 137994Tempol

생성물 1

HCID 10131000627085-11-4

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-9d6c42c37ccf421799e7048923e2e342
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07825134B2

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