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Benzoyl Peroxide → HCID 14653263, 화합물

HRID 893313
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HRID 893313 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[N:10]=[C:9]1[CH3:18].[Br:19]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)Cl>[Br:19][C:16]1[S:17][C:11]2[N:10]=[C:9]([CH3:18])[N:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[C:13](=[O:14])[C:12]=2[CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 9015653-(2-chlorophenyl)-2-methylthieno[2,3-d]pyrimidin-4(3H)-one

생성물 1

HCID 14653263HCID 14653263, 화합물수율 78.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

In chloroform was dissolved 22.85 g of 3,4-dihydro-3-(2-chlorophenyl)-2-methyl-4-oxothieno[2,3-d]pyrimidine, and 19.5 g of N-bromosuccinimide and trace benzoyl peroxide were added to the solution. The mixture was refluxed for 10 hours. After the resulting crystals were removed from the reaction mixture, the solvent was distilled off. The residue was crystallized from hexane-ethyl acetate to give 22.95 g of 3,4-dihydro-6-bromo-3-(2-chlorophenyl)-2-methyl-4-oxothieno[2,3-d]pyrimidine, m.p. 164.5°-166.5° C.

후처리

  1. additionwere added to the solution
  2. temperatureThe mixture was refluxed for 10 hours
  3. customAfter the resulting crystals were removed from the reaction mixture
  4. distillationthe solvent was distilled off
  5. customThe residue was crystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-8a68d65cb4ef46f6b5eea3eff7707541
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05124331

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