Acetyl chloride → (E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]acetamide

HRID 582209ノート

反応式

HRID 582209 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8]/[C:9]/2=[CH:12]\[CH2:13][NH2:14])=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:22](Cl)(=[O:24])[CH3:23]>O1CCCC1.O>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8]/[C:9]/2=[CH:12]\[CH2:13][NH:14][C:22](=[O:24])[CH3:23])=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 10987044(E)-1-(2-Aminoethylidene)-6-methoxyindan

生成物 1

HCID 59957023(E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]acetamide収率 111.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (E)-2-(6-methoxyindan-1-ylidene)-ethylamine (736 mg, 3.89 mmol) and triethylamine (0.59 g, 5.84 mmol) in tetrahydrofuran (20 ml) was added acetyl chloride (0.37 g, 4.70 mmol) gradually dropwise on an ice bath and the mixture was stirred at room temperature for 2 hours. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed serially with saturated saline and water and dried over anhydrous magnesium sulfate. Finally the solvent was distilled off under reduced pressure to provide (E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]acetamide (yield 1.0 g, 90%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed serially with saturated saline and water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationFinally the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-5e947cf76d3e4318a1128ef636fff228
出典データセット
uspto-grants-1999_07
特許番号
US05922771

反応ノート

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