Trichloroacetyl isocyanate → 7-Methylthieno[3,2-d]pyrimidine-2,4(1H,3H)-dione

HRID 1773513

반응식

HRID 1773513 반응식
Cl[C:2](Cl)(Cl)[C:3]([N:5]=[C:6]=[O:7])=[O:4].[NH2:10][C:11]1[C:15]([CH3:16])=[CH:14][S:13]C=1C(OC)=O>C(#N)C>[CH3:16][C:15]1[C:11]2[NH:10][C:6](=[O:7])[NH:5][C:3](=[O:4])[C:2]=2[S:13][CH:14]=1

참가 물질

4

반응물 2

HCID 76400Trichloroacetyl isocyanateHCID 123584Methyl 3-amino-4-methylthiophene-2-carboxylate

생성물 1

HCID 103523177-Methylthieno[3,2-d]pyrimidine-2,4(1H,3H)-dione수율 57.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
70 °C

실험 절차

Trichloroacetyl isocyanate (2.0 g) was added to a solution of methyl 3-amino-4-methylthiophene-2-carboxylate (1.3 g) in acetonitrile (10 mL) and the resulting mixture was stirred for 15 minutes. The solid, which crashed out, was collected by filtration and suspended in methanol (5 mL), a solution of ammonia in methanol (7 M, 5 mL) was then added and the resulting mixture was heated at 70° C. for 15 minutes. The reaction mixture was cooled, the solid formed was collected by filtration, dried under reduced pressure to give 0.8 g of 7-methyl-1H-thieno[3,2-d]pyrimidine-2,4-dione.

후처리

  1. filtrationwas collected by filtration
  2. additiona solution of ammonia in methanol (7 M, 5 mL) was then added
  3. temperatureThe reaction mixture was cooled
  4. customthe solid formed
  5. filtrationwas collected by filtration
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-218b4a2c57344b62b9fb03efb34e62c9
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09255110B2

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