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Water → N-(3,4-dichlorophenyl)-3-nitro-2-piperid-1-yl-5-trifluoromethylbenzamide

HRID 550349
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인쇄 미리보기

반응식

HRID 550349 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:25])[C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[CH:14]=[C:13]([N+:21]([O-:23])=[O:22])[C:12]=2Cl)[CH:5]=[CH:6][C:7]=1[Cl:8].[NH:26]1[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]1.O>O1CCOCC1.C(OCC)C.CCCCCC>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:25])[C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[CH:14]=[C:13]([N+:21]([O-:23])=[O:22])[C:12]=2[N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
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참가 물질

7

반응물 3

HCID 962WaterHCID 8082PiperidineHCID 86620253N-(3,4-dichlorophenyl)-2-chloro-3-nitro-5-trifluoromethylbenzamide

생성물 1

HCID 11854386N-(3,4-dichlorophenyl)-3-nitro-2-piperid-1-yl-5-trifluoromethylbenzamide

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 8058
Hexane
용매
HCID 312751,4-Dioxane용매

반응 조건

온도
25 °C

실험 절차

To a solution of N-(3,4-dichlorophenyl)-2-chloro-3-nitro-5-trifluoromethylbenzamide (0.76 g; 1 eq.) in dioxane (12 ml) is added piperidine (0.4 ml; 2.2 eq.). After stirring for 18 hours at 25° C., 10 ml of water are added and the product is extracted with ethyl acetate. The organic phase is dried and concentrated. The orange oil obtained is dissolved in 2 ml of ethyl ether and 120 ml of hexane. After 3 days at 0° C., the solid is filtered off by suction and dried. 540 mg of N-(3,4-dichlorophenyl)-3-nitro-2-piperid-1-yl-5-trifluoromethylbenzamide are obtained (m.p.=144° C.).

후처리

  1. extractionthe product is extracted with ethyl acetate
  2. customThe organic phase is dried
  3. concentrationconcentrated
  4. customThe orange oil obtained
  5. waitAfter 3 days at 0° C.
  6. filtrationthe solid is filtered off by suction
  7. customdried

출처 및 근거

ORD 기록
ord-7348f71b401b49b7b8cf85ea219973b1
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947675B2

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