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4-Amino-3-methylbenzamide → HCID 67176382, 화합물

HRID 709188
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HRID 709188 반응식
O=[C:2]([CH2:10][CH2:11][C:12](=O)[C:13]1[CH:18]=[CH:17][C:16]([N:19]2[CH2:23][CH2:22][O:21][C:20]2=[O:24])=[CH:15][CH:14]=1)[CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[NH2:26][C:27]1[CH:35]=[CH:34][C:30]([C:31]([NH2:33])=[O:32])=[CH:29][C:28]=1[CH3:36]>CCO.C(S([O-])(=O)=O)(F)(F)F.C(S([O-])(=O)=O)(F)(F)F.[Zn+2]>[C:31]([C:30]1[CH:34]=[CH:35][C:27]([N:26]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([N:19]4[CH2:23][CH2:22][O:21][C:20]4=[O:24])=[CH:15][CH:14]=3)=[CH:11][CH:10]=[C:2]2[CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[C:28]([CH3:36])[CH:29]=1)(=[O:32])[NH2:33]
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참가 물질

5

반응물 2

HCID 121180574-Amino-3-methylbenzamideHCID 67173612HCID 67173612, 화합물

생성물 1

HCID 67176382HCID 67176382, 화합물수율 39%

시약·촉매·용매 2

HCID 104671Zinc trifluoromethanesulfonate촉매HCID 702Ethanol용매

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온도
120 °C

실험 절차

To a solution of ethyl 4,7-dioxo-7-(4-(2-oxooxazolidin-3-yl)phenyl)heptanoate (158 mg, 0.43 mmol) and 4-amino-3-methylbenzamide (130 mg, 0.68 mmol) in EtOH (1 mL) was added Zn(OTf)2 (313 mg, 0.86 mmoL). The mixture was heated to 120° C. under microwave for 2 h. After evaporation under reduced pressure, the crude product was purified by silica gel column chromatography (DCM:MeOH=20:1) to afford the titled compound as a yellow solid (77 mg, yield 39%).

후처리

  1. customAfter evaporation under reduced pressure
  2. customthe crude product was purified by silica gel column chromatography (DCM:MeOH=20:1)

출처 및 근거

ORD 기록
ord-c9ba7e4df66744628fdd7389111817c5
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09180119B2

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