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

HRID 582209노트

반응식

HRID 582209 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5e947cf76d3e4318a1128ef636fff228
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922771

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