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

HRID 1773513

反応式

HRID 1773513 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-218b4a2c57344b62b9fb03efb34e62c9
出典データセット
uspto-grants-2016_02
特許番号
US09255110B2

関連ノート

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