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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
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HRID 1485493 반응식
[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
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참가 물질

4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e3c7efbe813a423ba90311c9f021cc32
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422307B2

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