Ethyl Bromide → 3-ethyl-1-(4-nitrophenyl)-2,4(1H,3H)-pyrimidinedione

HRID 2106764

반응식

HRID 2106764 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH:15]=[CH:14][C:13](=[O:16])[NH:12][C:11]2=[O:17])=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH-].[K+].Br[CH2:21][CH3:22]>CN(C)C(=O)C>[CH2:21]([N:12]1[C:13](=[O:16])[CH:14]=[CH:15][N:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[C:11]1=[O:17])[CH3:22]

참가 물질

5

반응물 3

HCID 6332Ethyl BromideHCID 14797Potassium HydroxideHCID 112763381-(4-Nitrophenyl)pyrimidine-2,4-dione

생성물 1

HCID 151254793-ethyl-1-(4-nitrophenyl)-2,4(1H,3H)-pyrimidinedione수율 65.6%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A mixture of 3 parts of 1-(4-nitrophenyl)-2,4(1H,3H)-pyrimidinedione, 1,4 parts of potassium hydroxide and 67.5 parts of N,N-dimethylacetamide was stirred for 1 hour at room temperature under nitrogen atmosphere. 1.52 Parts of bromoethane were added and stirring was continued overnight at room temperature. The reaction mixture was poured into 100 parts of ice water. The product was filtered off and stirred in methanol. The product was filtered off and dried in vacuo at 60° C., yielding 2.4 parts (65.6%) of 3-ethyl-1-(4-nitro-phenyl)-2,4(1H,3H)-pyrimidinedione; mp. 182.5° C. (int. 24).

후처리

  1. stirringstirring
  2. waitwas continued overnight at room temperature
  3. filtrationThe product was filtered off
  4. stirringstirred in methanol
  5. filtrationThe product was filtered off
  6. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-d072a9a384e947f2a9bfee02dda21a87
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04931444

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