Hydrazine hydrate (1:1) → HCID 178515597, 화합물

HRID 2182810노트

반응식

HRID 2182810 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=O)[CH2:10][C:11]([O:13]C)=O.O.[NH2:17][NH2:18]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:10]=[C:11]([OH:13])[NH:18][N:17]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 2758178Methyl 3-(2,4-dichlorophenyl)-3-oxopropanoate

생성물 1

HCID 178515597HCID 178515597, 화합물수율 79.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

970 g of methyl 3-(2,4-dichlorophenyl)-3-oxopropionate were initially charged in 4000 ml of ethanol. Over a period of 15 min, 201 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 filtrate 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 714.2 g (79.4%) of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole as a colorless solid. M.p.: 198° C.

후처리

  1. filtrationthe precipitated solid was filtered off
  2. concentrationthe filtrate was concentrated
  3. stirringThe filtrate 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-a8803a72fbbd4cc6931c2e25f163882e
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897322B2

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