Acetic Acid → 1-Benzyl-5-benzylidene-3-phenylbarbituric acid

HRID 1774089

반응식

HRID 1774089 반응식
[CH2:1]([N:8]1[C:15](=[O:16])[CH2:14][C:12](=[O:13])[N:11]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:23](=O)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(O)(=O)C.S(=O)(=O)(O)O>O.C(O)(C)C>[CH2:1]([N:8]1[C:15](=[O:16])[C:14](=[CH:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:12](=[O:13])[N:11]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 240BenzaldehydeHCID 1118Sulfuric AcidHCID 217087511-Benzyl-3-phenylbarbituric acid

생성물 1

HCID 867308661-Benzyl-5-benzylidene-3-phenylbarbituric acid수율 75%

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

반응 조건

온도
50 °C

실험 절차

In a 300-ml glass flask equipped with a thermometer, a reflux condenser and a stirrer, 4.0 g of 1-benzyl-3-phenylbarbituric acid, 1.6 g of benzaldehyde, and 40 ml of acetic acid were put, the content was added with a drop of sulfuric acid, kept under stirring, the flask was heated so as to adjust the inner temperature to 100° C., and the content was continued to be stirred at 100° C. for 3 hours. The content was then cooled to 50° C., added with a mixed solution of 39 ml of isopropanol and 17 ml of water, stirred at 10° C. or below for one hour, filtered under suction to collect a deposited crystal, and the crystal was washed with methanol, to thereby obtain 3.9 g of 1-benzyl-5-benzylidene-3-phenylbarbituric acid as an intermediate.

후처리

  1. temperaturethe flask was heated so as
  2. customto 100° C.
  3. stirringto be stirred at 100° C. for 3 hours
  4. stirringstirred at 10° C. or below for one hour
  5. filtrationfiltered under suction
  6. customto collect a deposited crystal
  7. washthe crystal was washed with methanol

출처 및 근거

ORD 기록
ord-29891404cbbb493095dee0f31f8f76ec
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09256099B2

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