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Ethyl benzoylacetate → 2-amino-6-phenyl-4H-1,3-oxazin-4-one

HRID 2413028
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HRID 2413028 반응식
C[NH:2][C:3](=[NH:5])S.OS(O)(=O)=O.[OH-].[K+].[C:13]([CH2:21][C:22]([O:24]CC)=O)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>O>[NH2:5][C:3]1[O:20][C:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:21][C:22](=[O:24])[N:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7170Ethyl benzoylacetateHCID 14797Potassium HydroxideHCID 178485225HCID 178485225, 화합물

생성물 1

HCID 133709342-amino-6-phenyl-4H-1,3-oxazin-4-one수율 76.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 9.45 g (0.034 M) of methylthiopseudourea H2SO4 is added 40.0 ml of H2O+8.0 g (0.142 M) of KOH. With vigorous stirring, 12.0 g (0.0625 M) of ethyl benzoylacetate (Aldrich) is also added and the heterogenous mixture allowed to stir at ambient temperature for 18 hours. The resulting solids are filtered and washed very well with H2O followed by ether. The solids are dried at 60° C. in a vacuum oven to yield 7.20 g (61.3 percent) of 2-amino-6-phenyl-1,3-oxazine-4-one. An analytical sample is recrystallized from 95 percent EtOH:DMF to yield 2-amino-6-phenyl-1,3-oxazine-4-one (m.p. 244-246 d).

후처리

  1. filtrationThe resulting solids are filtered
  2. washwashed very well with H2O
  3. customThe solids are dried at 60° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-839c982fd00b4b24b8b7150b2a0c6295
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04495349

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