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Hydrazine hydrate (1:1) → HCID 14951339, 화합물

HRID 973954
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반응식

HRID 973954 반응식
O.[NH2:2][NH2:3].[Cl:4][C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[C:7]([Cl:12])[C:6]=1[NH:13][C:14]1[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=1[C:16](OC)=[O:17]>CO>[Cl:4][C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[C:7]([Cl:12])[C:6]=1[NH:13][C:14]1[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=1[C:16]([NH:2][NH2:3])=[O:17]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 76743Benzoic acid, 2-((2,6-dichloro-3-methylphenyl)amino)-, methyl ester

생성물 1

HCID 14951339HCID 14951339, 화합물수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

Hydrazine hydrate (2 ml) is added dropwise to a suspension of methyl 2-[(2,6-dichloro-3-methylphenyl)amino]-benzoate (227.1 mg, .73 mmol) in 10 ml of methanol. The reaction mixture is heated at 60° C for seven hours under an atmosphere of nitrogen and then allowed to cool to room temperature overnight. The now clear colorless solution is concentrated in vacuo and chromatographed, eluting with ethyl acetate and hexane (gradient of 1:2 to 1:1), providing 208.6 mg (92%) of a white solid, mp 158°-160° C.

후처리

  1. temperatureto cool to room temperature overnight
  2. concentrationThe now clear colorless solution is concentrated in vacuo
  3. customchromatographed
  4. washeluting with ethyl acetate and hexane (gradient of 1:2 to 1:1)

출처 및 근거

ORD 기록
ord-f23f884631cb4b71b456d367c6232979
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05066668

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