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Sodium Hydroxide → 4-[4-[2-[(methylsulfonyl)methyl]-1H-imidazol-1-yl]butyl]phenol

HRID 1610952
ノート
印刷プレビュー

反応式

HRID 1610952 の反応式
[OH:1]OS([O-])=O.[K+].[CH3:7][S:8][CH2:9][C:10]1[N:11]([CH2:15][CH2:16][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=2)[CH:12]=[CH:13][N:14]=1.[OH-:26].[Na+]>CO.O>[CH3:7][S:8]([CH2:9][C:10]1[N:11]([CH2:15][CH2:16][CH2:17][CH2:18][C:19]2[CH:20]=[CH:21][C:22]([OH:25])=[CH:23][CH:24]=2)[CH:12]=[CH:13][N:14]=1)(=[O:1])=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 222593474-[4-[2-[(methylthio)methyl]-1H-imidazol-1-yl]butyl]phenolHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 222592974-[4-[2-[(methylsulfonyl)methyl]-1H-imidazol-1-yl]butyl]phenol

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

Oxone (Trade mark; potassium peroxymonosulfate: 28.8 g) was added to a suspension of 4-[4-[2-[(methylthio)methyl]-1H-imidazol-1-yl]butyl]phenol (8.64 g) in methanol-water (2:1) (150 ml) at 0° C. and the mixture was stirred at room temperature for 3.5 hr. The reaction mixture was adjusted to pH 6 by addition of 4N aqueous sodium hydroxide solution to precipitate crystals, which were collected by filtration. The crystals were dissolved in ethyl acetate-methanol (1:4), and the insoluble was filtered off. The filtrated was concentrated and recrystallized from ethyl acetate-methanol-hexane to give the titled compound (6.53 g) as colorless needle crystals.

後処理

  1. customto precipitate crystals, which
  2. filtrationwere collected by filtration
  3. dissolutionThe crystals were dissolved in ethyl acetate-methanol (1:4)
  4. filtrationthe insoluble was filtered off
  5. concentrationThe filtrated was concentrated
  6. customrecrystallized from ethyl acetate-methanol-hexane

出典と根拠

ORDレコード
ord-db391cbd504b442b8a212870d70892af
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06984653B2

反応ノート

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