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2-[N-methyl-N-(4-nitrophenyl)amino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one → HCID 23287606, 화합물

HRID 367187
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HRID 367187 반응식
[CH3:1][N:2]([C:12]1[S:13][C:14]2[N:22]=[CH:21][CH:20]=[CH:19][C:15]=2[C:16](=[O:18])[N:17]=1)[C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-])=[O:10])=[CH:5][CH:4]=1.[H][H]>[Pd].CN(C=O)C>[OH:10][NH:9][C:6]1[CH:7]=[CH:8][C:3]([N:2]([C:12]2[S:13][C:14]3[N:22]=[CH:21][CH:20]=[CH:19][C:15]=3[C:16](=[O:18])[N:17]=2)[CH3:1])=[CH:4][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 232877462-[N-methyl-N-(4-nitrophenyl)amino]-4H-pyrido[3,2-e]-1,3-thiazin-4-oneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 23287606HCID 23287606, 화합물수율 6.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1.181 g (3.76 mmol) of 2-[N-methyl-N-(4-nitrophenyl)amino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one obtained in Example 63, 100 ml of DMF and 250 mg of 10% Pd on carbon was stirred in an atmosphere of hydrogen for 6 days. The reaction mixture was then heated so that the compound thus precipitated was dissolved. The insoluble matters were hot-removed by filtration. The solution thus obtained was then allowed to cool to room temperature. The resulting crystal was collected by filtration, washed with THF and then with ethanol, and then dried under reduced pressure to obtain 77 mg of 2-[N-(4-hydroxyaminophenyl)-N-methylamino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one.

후처리

  1. temperatureThe reaction mixture was then heated so that the compound
  2. customthus precipitated
  3. dissolutionwas dissolved
  4. customThe insoluble matters were hot-removed by filtration
  5. customThe solution thus obtained
  6. filtrationThe resulting crystal was collected by filtration
  7. washwashed with THF
  8. dry with materialwith ethanol, and then dried under reduced pressure

출처 및 근거

ORD 기록
ord-9b1cd0e997d448b58b0067e5c8070d80
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06133258

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