2-Chloro-5-nitrobenzyl alcohol → 3-Hydroxymethyl-4-(methylthio)nitrobenzene

HRID 396811

反応式

HRID 396811 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH2:11][OH:12].C(S)[CH2:14][S:15]([O-])(=O)=O.[Na+]>CS(C)=O.CO>[OH:12][CH2:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[S:15][CH3:14]

参加物

5

反応物 2

HCID 5557222-Chloro-5-nitrobenzyl alcoholHCID 23662354Mesna

生成物 1

HCID 223168073-Hydroxymethyl-4-(methylthio)nitrobenzene収率 105.4%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 887Methanol溶媒

実験手順

To a solution of 4-chloro-3-(hydroxymethyl)nitrobenzene (20 g, 0.10 mol) in DMSO (160 mL) and MeOH (80 mL), MeSNa (8.2 g, 0.12 mol) was added portionwise at 0° C., and the mixture was stirrred for 2 h at room temperature. The mixture was poured into ice water (300 mL) and the yellow precipitate was collected by filtration and washed with ether (150 mL) gave the title compound (21 g, quantitative).

後処理

  1. filtrationthe yellow precipitate was collected by filtration
  2. washwashed with ether (150 mL)

出典と根拠

ORDレコード
ord-566669d76c614695a16237762494fd90
出典データセット
uspto-grants-2003_08
特許番号
US06608095B2

関連ノート

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