Pyridine → (3AS-cis)-1,3-Dibenzyltetrahydro-1H-thieno[3,4-D]imidazole-2,4-dione

HRID 1715789ノート

反応式

HRID 1715789 の反応式
[CH2:1]([N:8]1[C@H:12]2[CH2:13][S:14][C:15](=[O:16])[C@@H:11]2[N:10]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:9]1=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C=CC=CC=1>C(Cl)(Cl)Cl>[CH2:1]([N:8]1[C@H:12]2[CH2:13][S:14][C:15](=[O:16])[C@H:11]2[N:10]([CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:9]1=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 1049PyridineHCID 86596559(3aR,6aR)-1,3-dibenzyl-hexahydro-4H-thieno[3,4-d]imidazol-2,4-dione

生成物 1

HCID 119817(3AS-cis)-1,3-Dibenzyltetrahydro-1H-thieno[3,4-D]imidazole-2,4-dione収率 75.1%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 1 ml of chloroform was dissolved 100 mg of (3aR,6aR)-1,3-dibenzyl-hexahydro-4H-thieno[3,4-d]imidazol-2,4-dione, 0.5 ml of pyridine was added to the solution, and the resulting mixture was stirred at room temperature for 23 hours. The reaction mixture was successively washed with 2M hydrochloric acid, water, a saturated sodium bicarbonate solution, and saturated brine. The organic layer was dried and then concentrated. By adding isopropyl ether, precipitated crystal was collected by filtration to give 75.1 mg of (3aS,6aR)-1,3-dibenzyl-hexahydro-4H-thieno[3,4-d]imidazol-2,4-dione.

後処理

  1. additionwas added to the solution
  2. washThe reaction mixture was successively washed with 2M hydrochloric acid, water
  3. customThe organic layer was dried
  4. concentrationconcentrated
  5. additionBy adding isopropyl ether
  6. customprecipitated crystal
  7. filtrationwas collected by filtration

出典と根拠

ORDレコード
ord-9c6eee4c895c4330a9d80843509f62f2
出典データセット
uspto-grants-2010_09
特許番号
US07799929B2

反応ノート

読み込み中…