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Water → N-((4-chloromethyl-2,6-dimethylphenyl)methyl)acetamide

HRID 1282064
ノート
印刷プレビュー

反応式

HRID 1282064 の反応式
O[CH2:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([CH2:10][NH:11][C:12](=[O:14])[CH3:13])=[C:5]([CH3:15])[CH:4]=1.S(Cl)([Cl:18])=O.O>ClCCl>[Cl:18][CH2:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([CH2:10][NH:11][C:12](=[O:14])[CH3:13])=[C:5]([CH3:15])[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

5

反応物 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 18423136N-((4-hydroxymethyl-2,6-dimethylphenyl)methyl)acetamide

生成物 1

HCID 18423130N-((4-chloromethyl-2,6-dimethylphenyl)methyl)acetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of N-((4-hydroxymethyl-2,6-dimethylphenyl)methyl)acetamide (1.0 g) in dichloromethane (12 ml) was added thionyl chloride (0.88 ml). This mixture was stirred at room temperature for 3 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with aqueous sodium hydrogencarbonate and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was recrystallized from ethyl acetate-isopropyl ether to give the title compound (1.0 g) as white crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with aqueous sodium hydrogencarbonate and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe obtained residue was recrystallized from ethyl acetate-isopropyl ether

出典と根拠

ORDレコード
ord-1de72c86f6dc48e18196c7cebf295018
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455528B1

反応ノート

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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