Potassium Carbonate → HCID 53982614, 화합물

HRID 1073239노트

반응식

HRID 1073239 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 660233-Phenylprop-2-enoyl chlorideHCID 22379525HCID 22379525, 화합물

생성물 1

HCID 53982614HCID 53982614, 화합물수율 95.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7c9ee856e5024ae5bd46cad6cd0e2413
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968698

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