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

HRID 1511596

反応式

HRID 1511596 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-08eb0dac5f7d41f381ee68cbddfad073
出典データセット
uspto-grants-2012_07
特許番号
US08217031B2

関連ノート

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