Potassium Carbonate → HCID 53982614、化合物

HRID 1073239ノート

反応式

HRID 1073239 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH2:12][CH2:13][NH2:14])[CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4].C(=O)([O-])[O-].[K+].[K+].[C:21](Cl)(=[O:30])[CH:22]=[CH:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(#N)C>[C:24]1([CH:23]=[CH:22][C:21]([NH:14][CH2:13][CH2:12][C:8]2[CH:9]=[CH:10][CH:11]=[C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])[CH:7]=2)=[O:30])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 660233-Phenylprop-2-enoyl chlorideHCID 22379525HCID 22379525、化合物

生成物 1

HCID 53982614HCID 53982614、化合物収率 95.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 2-(3-butyloxyphenyl)ethylamine (1.0 g) in acetonitrile (40 cm3) was added powdered potassium carbonate (0.80 g). Cinnamoyl chloride (1.03 g) was then added portionwise over a period of fifteen minutes and the reaction mixture was then stirred at room temperature for 6.5 hours after which distilled water (40 cm3) was added. The mixture was left to stand overnight and was then filtered and extracted several times with ethyl acetate. The combined ethyl acetate extracts were washed successively with potassium bicarbonate solution, water and 0.5M hydrochloric acid before drying over sodium sulphate and then evaporating down to give the product as a tan coloured oil (1.60 g).

後処理

  1. distillationdistilled water (40 cm3)
  2. additionwas added
  3. waitThe mixture was left
  4. waitto stand overnight
  5. filtrationwas then filtered
  6. extractionextracted several times with ethyl acetate
  7. washThe combined ethyl acetate extracts were washed successively with potassium bicarbonate solution, water and 0.5M hydrochloric acid
  8. dry with materialbefore drying over sodium sulphate
  9. customevaporating down

出典と根拠

ORDレコード
ord-7c9ee856e5024ae5bd46cad6cd0e2413
出典データセット
uspto-grants-1990_11
特許番号
US04968698

反応ノート

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