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2,N-Dimethylaniline → 4-(2,5-Dichloro-phenoxy)-N-methyl-N-o-tolyl-nicotinamide

HRID 1025833
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HRID 1025833 반응식
[Cl:1][C:2]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][C:6]=1[C:11]([N:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16]C[CH2:14]1)=[O:12].CNC1C(C)=CC=CC=1>CCCCCCC.C(OCC)(=O)C>[Cl:1][C:2]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:3]=1[O:4][C:5]1[C:6]([C:11]([N:13]([CH3:14])[C:22]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:16])=[O:12])=[CH:7][N:8]=[CH:9][CH:10]=1
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참가 물질

4

반응물 2

HCID 691372,N-DimethylanilineHCID 53311781[4-(2,5-Dichloro-phenoxy)-pyridin-3-yl]-(3,4-dihydro-2H-quinolin-1-yl)-methanone

생성물 1

HCID 461945684-(2,5-Dichloro-phenoxy)-N-methyl-N-o-tolyl-nicotinamide

시약·촉매·용매 1

HCID 21899848Ethylacetate heptane용매

실험 절차

The title compound was prepared in analogy to Example 1, from 4-(2,5-dichloro-phenoxy)-nicotinic acid (Example 1, intermediate) and N-methyl-o-toluidine (commercially available; CAS RN 611-21-2) and using a gradient of n-heptane:ethyl acetate (100:0 to 40:60). The compound was further purified through a second preparative HPLC chromatography (Phenomenex Gemini column) using a gradient of acetonitrile:water (containing 0.05% formic acid) (10:90 to 98:2). White solid (35%). MS (ESI): m/z=387.066 [M+H]+.

후처리

  1. customThe compound was further purified through a second preparative HPLC chromatography (Phenomenex Gemini column)

출처 및 근거

ORD 기록
ord-714df8a0763642d98acb2f5fe30e94e1
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729091B2

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