Ammonia → 4,5,6,7-Tetrahydrothieno[2,3-c]pyridin-4-ol

HRID 1511596

반응식

HRID 1511596 반응식
C([O:3][CH:4](OCC)[CH2:5][NH:6][CH2:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)C.N>Cl>[S:9]1[C:8]2[CH2:7][NH:6][CH2:5][CH:4]([OH:3])[C:12]=2[CH:11]=[CH:10]1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 27953962,2-diethoxy-N-(thiophen-2-ylmethyl)ethanamine

생성물 1

HCID 123370234,5,6,7-Tetrahydrothieno[2,3-c]pyridin-4-ol수율 28.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

2,2-Diethoxy-N-(thiophen-2-ylmethyl)ethaneamine (72.5 g) prepared in the step 2 was dissolved in 5N aqueous solution of hydrochloric acid and stirred overnight at room temperature. The reaction solution was neutralized with 10% aqueous ammonia and subjected to extraction with ethyl acetate. The organic layer was separated, washed with water and a saturated solution of sodium chloride successively, dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo. The residue was purified by silica gel column chromatography to give 14.0 g of the objective compound.

후처리

  1. extractionsubjected to extraction with ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materiala saturated solution of sodium chloride successively, dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-08eb0dac5f7d41f381ee68cbddfad073
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217031B2

연결된 노트

불러오는 중…