Hydrazine hydrate (1:1) → HCID 178515597、化合物

HRID 2182810ノート

反応式

HRID 2182810 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178515597HCID 178515597、化合物収率 79.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a8803a72fbbd4cc6931c2e25f163882e
出典データセット
uspto-grants-2005_05
特許番号
US06897322B2

反応ノート

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