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Stannous chloride dihydrate → 7-(3-aminophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine

HRID 1485493
ノート
印刷プレビュー

反応式

HRID 1485493 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[C:14]3[N:15]=[C:16]([NH:20][C:21]4[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[C:23]([O:31][CH3:32])[CH:22]=4)[N:17]=[C:18]([NH2:19])[C:13]=3[S:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1)([O-])=O.O.O.[Sn](Cl)Cl>C(O)C>[NH2:1][C:4]1[CH:5]=[C:6]([C:10]2[C:14]3[N:15]=[C:16]([NH:20][C:21]4[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[C:23]([O:31][CH3:32])[CH:22]=4)[N:17]=[C:18]([NH2:19])[C:13]=3[S:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 672038457-(3-Nitrophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine

生成物 1

HCID 532379637-(3-aminophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine収率 85.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

7-(3-Nitrophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine (400 mg, 0.88 mmol) was dissolved in ethanol (3.0 mL) and tin(II) chloride dihydrate (996 mg, 4.41 mmol) was added. The reaction mixture was stirred at 80° C. for 2 hours. After removing ethanol by distillation under reduced pressure, ammonia water was slowly added to make pH 5. Sodium carbonate was added to thus prepared yellow precipitate until the pH reached 7. The precipitate was filtered and washed several times with ethyl acetate. Concentration of the filtrate yielded the target compound of Example 11 (320 mg, 85% yield).

後処理

  1. customAfter removing ethanol
  2. distillationby distillation under reduced pressure, ammonia water
  3. additionwas slowly added
  4. additionSodium carbonate was added to thus prepared yellow precipitate until the pH
  5. filtrationThe precipitate was filtered
  6. washwashed several times with ethyl acetate

出典と根拠

ORDレコード
ord-e3c7efbe813a423ba90311c9f021cc32
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09422307B2

反応ノート

読み込み中…

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