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Hydrazine hydrate (1:1) → HCID 178515601, 화합물

HRID 2182805
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HRID 2182805 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10](OCC)=[O:11])=[C:4]([F:16])[CH:3]=1.O.[NH2:18][NH2:19]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[C:10]([OH:11])[NH:19][N:18]=2)=[C:4]([F:16])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 11195926Ethyl 3-(4-chloro-2-fluorophenyl)-3-oxopropanoate

생성물 1

HCID 178515601HCID 178515601, 화합물수율 77.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

428.4 g of ethyl 3-(4-chloro-2-fluorophenyl)-3-oxopropionate were initially charged in 1400 ml of ethanol. Over a period of 15 min, 92 g of hydrazine hydrate were added dropwise, the mixture was stirred at room temperature overnight, the precipitated solid was filtered off and the filtrate was concentrated to ⅓ of its original volume. The mixture was stirred for another two nights, the resulting solid was filtered off with suction and the filtrate was again concentrated to ⅓ of its original volume. This gave a total of 289.1 g (77.7%) of 3-(4-chloro-2-fluorophenyl)-5-hydroxy-1H-pyrazole as a colorless solid. M.p.: 194° C.

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후처리

  1. filtrationthe precipitated solid was filtered off
  2. concentrationthe filtrate was concentrated
  3. stirringThe mixture was stirred for another two nights
  4. filtrationthe resulting solid was filtered off with suction
  5. concentrationthe filtrate was again concentrated

출처 및 근거

ORD 기록
ord-bba5b1c3d3404caeb8cb53370bd9c065
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06897322B2

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