Methyl acetoacetate → HCID 178463089、化合物

HRID 350875

反応式

HRID 350875 の反応式
C(O)(=O)C(O)=O.[CH2:7]([NH:9][NH2:10])[CH3:8].C(N(CC)CC)C.[C:18](OC)(=[O:23])[CH2:19][C:20]([CH3:22])=O>C1(C)C=CC=CC=1>[CH2:7]([N:9]1[C:18]([OH:23])=[CH:19][C:20]([CH3:22])=[N:10]1)[CH3:8]

参加物

5

反応物 3

HCID 7757Methyl acetoacetateHCID 8471TriethylamineHCID 96181Hydrazine, ethyl-, ethanedioate (1:1)

生成物 1

HCID 178463089HCID 178463089、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 3.9 g of ethyl hydrazine oxalate and 3.6 ml of triethylamine in 80 ml of toluene was stirred at room temperature for 15 min. 2.8 ml of methyl acetoacetate was added and the mixture was azeotroped for 1.5 h. The mixture was evaporated and the residue was purified by flash chromatography on silica gel using dichloromethane/methanol (97:3) for the elution to give 3.1 g of 2-ethyl-5-methyl-2H-pyrazol-3-ol as an orange solid.

後処理

  1. customthe mixture was azeotroped for 1.5 h
  2. customThe mixture was evaporated
  3. customthe residue was purified by flash chromatography on silica gel
  4. washfor the elution

出典と根拠

ORDレコード
ord-6d1a392d47f548fd945ce90ac47d6138
出典データセット
uspto-grants-2007_02
特許番号
US07183296B2

関連ノート

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