ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 4-bromo-2-ethyl-5-(4-methoxymethoxybenzyloxy)-3(2H)-pyridazinone

HRID 1904236
ノート
印刷プレビュー

反応式

HRID 1904236 の反応式
[Br:1][C:2]1[C:3](=[O:11])[N:4]([CH2:9][CH3:10])[N:5]=[CH:6][C:7]=1Br.[CH3:12][O:13][CH2:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][OH:21])=[CH:18][CH:17]=1.[OH-].[K+].O>CN(C)C=O>[Br:1][C:2]1[C:3](=[O:11])[N:4]([CH2:9][CH3:10])[N:5]=[CH:6][C:7]=1[O:21][CH2:20][C:19]1[CH:18]=[CH:17][C:16]([O:15][CH2:14][O:13][CH3:12])=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 106605064,5-Dibromo-2-ethylpyridazin-3(2H)-oneHCID 116079844-Methoxymethoxybenzylalcohol

生成物 1

HCID 146717974-bromo-2-ethyl-5-(4-methoxymethoxybenzyloxy)-3(2H)-pyridazinone収率 28.6%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

In 30 ml of N,N-dimethylformamide were dissolved 1.2 g of 4,5-dibromo-2-ethyl-3(2H)-pyridazinone and 0.88 g of 4-methoxymethoxybenzyl alcohol, and 0.34 g of powdery potassium hydroxide was added thereto. The reaction mixture was stirred overnight at room temperature, poured into water and extracted with benzene. The benzene layer was washed with water, dried over anhydrous sodium sulfate and freed of the benzene by distillation under reduced pressure. The resulting oil was purified by means of TLC [eluting with benzene/ethyl acetate (12/1)] and recrystallization (from benzene/n-hexane) to obtain 450 mg of the aimed compound, m.p. 104°~106.0° C.

後処理

  1. additionwas added
  2. extractionextracted with benzene
  3. washThe benzene layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationfreed of the benzene by distillation under reduced pressure
  6. customThe resulting oil was purified by means of TLC [eluting with benzene/ethyl acetate (12/1)] and recrystallization (from benzene/n-hexane)

出典と根拠

ORDレコード
ord-ce4576a8c8ff4514b0942948f62c4592
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04837217

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート