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Acetyl chloride → N-((4-hydroxymethyl-2,6-dimethylphenyl)methyl)acetamide

HRID 1282063
ノート
印刷プレビュー

反応式

HRID 1282063 の反応式
[NH2:1][CH2:2][C:3]1[C:10]([CH3:11])=[CH:9][C:6]([CH2:7][OH:8])=[CH:5][C:4]=1[CH3:12].C(=O)([O-])[O-].[K+].[K+].[C:19](Cl)(=[O:21])[CH3:20]>C(OCC)(=O)C.O>[OH:8][CH2:7][C:6]1[CH:9]=[C:10]([CH3:11])[C:3]([CH2:2][NH:1][C:19](=[O:21])[CH3:20])=[C:4]([CH3:12])[CH:5]=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 3

HCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 23383595[4-(Aminomethyl)-3,5-dimethylphenyl]methanol

生成物 1

HCID 18423136N-((4-hydroxymethyl-2,6-dimethylphenyl)methyl)acetamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-aminomethyl-3,5-dimethylbenzyl alcohol (2.3 g) in ethyl acetate (70 ml) was added a solution of potassium carbonate (2.0 g) in water (35 ml). To this solution was added acetyl chloride (0.95 ml) under ice-cooling. This mixture was stirred at room temperature for 1 hr. The reaction mixture was extracted with ethyl acetate, washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was recrystallized from methanol-ethyl acetate to give the title compound (2.0 g) as white crystals, m.p.=193.5-194.5° C.

後処理

  1. temperaturecooling
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe obtained residue was recrystallized from methanol-ethyl acetate

出典と根拠

ORDレコード
ord-31a2246e1d0d43958bb8a8d963dcdb21
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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