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3,5-Dichlorophenyl isocyanate → Ethyl 4-[(3,5-dichloroanilino)carbonyl]-2-piperazinecarboxylate

HRID 2414630
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인쇄 미리보기

반응식

HRID 2414630 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH:2]1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[Cl:12][C:13]1[CH:14]=[C:15]([N:20]=[C:21]=[O:22])[CH:16]=[C:17]([Cl:19])[CH:18]=1>C(Cl)(Cl)Cl>[Cl:12][C:13]1[CH:14]=[C:15]([CH:16]=[C:17]([Cl:19])[CH:18]=1)[NH:20][C:21]([N:4]1[CH2:5][CH2:6][NH:1][CH:2]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3]1)=[O:22]
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참가 물질

4

반응물 2

HCID 944603,5-Dichlorophenyl isocyanateHCID 10633257Ethyl Piperazine-2-carboxylate

생성물 1

HCID 22644956Ethyl 4-[(3,5-dichloroanilino)carbonyl]-2-piperazinecarboxylate수율 27%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of ethyl 2-piperazinecarboxylate (0.9 g, 5.7 mmol) in chloroform (11 mL) was added 3,5-dichlorophenyl isocyanate (1.05 g, 5.7 mmol). The reaction was stirred overnight after which time a precipitate had formed. The reaction was concentrated and the solid was chromatographed on silica gel using ethyl acetate as eluant to provide 0.53 g (27%) of ethyl 4-[(3,5-dichloroanilino)carbonyl]-2-piperazinecarboxylate as an off white powder. Electrospray Mass Spec 346.1 (M+H)+.

후처리

  1. customhad formed
  2. concentrationThe reaction was concentrated
  3. customthe solid was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-b8731ca2cadd49669d189196c1bb1a48
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06812227B2

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