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

Hydrogen Peroxide → HCID 12850099、化合物

HRID 973456
ノート
印刷プレビュー

反応式

HRID 973456 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH:11]([NH:13][CH2:14][CH:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[C:19]([S:24][CH3:25])[CH:18]=2)[OH:16])[CH3:12])=[CH:5][CH:4]=1.[OH:26]O>CO>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH:11]([NH:13][CH2:14][CH:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[C:19]([S:24]([CH3:25])=[O:26])[CH:18]=2)[OH:16])[CH3:12])=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 12850096HCID 12850096、化合物

生成物 1

HCID 12850099HCID 12850099、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 70 ml of methanol was dissolved 2.5 g of α-{[3-(4-methoxyphenyl)-1-methylpropylamino]-methyl}-4-methyl-3-methylthiobenzenemethanol and then 8 ml of an aqueous 30% hydrogen peroxide solution was added dropwise to the solution under ice-cooling. After allowing the reaction mixture to stand overnight the at room temperature, methanol was distilled off and after adding 50 ml of water to the residue, the product was extracted with ethyl acetate. The ethyl acetate layer formed was dried with anhydrous magnesium sulfate and after distilling off the solvent, the residue was purified by a silica gel column chromatography (eluate: a mixture of benzene, ethyl acetate, and methanol (4:3:1 by volume ratio) to provide 2.0 g of the amorphous caramel-like powder of α-{[3-(4-methoxyphenyl)-1-methylpropylamino]methyl}-4-methyl-3-methylsulfinylbenzenemethanol.

後処理

  1. temperaturecooling
  2. distillationthe at room temperature, methanol was distilled off
  3. additionafter adding 50 ml of water to the residue
  4. extractionthe product was extracted with ethyl acetate
  5. customThe ethyl acetate layer formed
  6. dry with materialwas dried with anhydrous magnesium sulfate
  7. distillationafter distilling off the solvent
  8. customthe residue was purified by a silica gel column chromatography (eluate
  9. additiona mixture of benzene, ethyl acetate, and methanol (4:3:1 by volume ratio)

出典と根拠

ORDレコード
ord-d9557991388e4b538570174d0a04f7af
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05063246

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