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

HRID 367187
ノート
印刷プレビュー

反応式

HRID 367187 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 23287606HCID 23287606、化合物収率 6.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9b1cd0e997d448b58b0067e5c8070d80
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133258

反応ノート

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