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

HRID 1715789노트

반응식

HRID 1715789 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c6eee4c895c4330a9d80843509f62f2
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07799929B2

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