Potassium Carbonate → 4-Hydroxy-6-mesyl-4,5,6,7-tetrahydro thieno[2,3-c]pyridine

HRID 2413129ノート

反応式

HRID 2413129 の反応式
Cl.[OH:2][CH:3]1[CH2:8][NH:7][CH2:6][C:5]2[S:9][CH:10]=[CH:11][C:4]1=2.C(=O)([O-])[O-].[K+].[K+].[CH3:18][S:19](Cl)(=[O:21])=[O:20]>C(Cl)(Cl)Cl>[OH:2][CH:3]1[CH2:8][N:7]([S:19]([CH3:18])(=[O:21])=[O:20])[CH2:6][C:5]2[S:9][CH:10]=[CH:11][C:4]1=2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 123370244,5,6,7-Tetrahydrothieno[2,3-c]pyridin-4-ol;hydrochloride

生成物 1

HCID 543441984-Hydroxy-6-mesyl-4,5,6,7-tetrahydro thieno[2,3-c]pyridine収率 76%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a mixture of 4-hydroxy-4,5,6,7-tetrahydro-thieno-[2,3-c]pyridine hydrochloride (50 g; 0.26 mole), chloroform (200 ml) and saturated aqueous potassium carbonate solution (100 ml) is added dropwise a solution of methanesulfonyl chloride (30 g; 0.26 mole) in chloroform (50 ml), at room temperature and with vigorous mechanical stirring. Stirring is continued a further 2 hours at room temperature. After decantation, the chloroform phase is washed with dilute hydrochloric acid, then with water, and is dried over anhydrous sodium sulfate. Evaporation of the solvent, in vacuo, leaves crystals which are recrystallized from methanol. Light brown crystals; M.p.=140° C. (methanol); Yield: 76%.

後処理

  1. customat room temperature
  2. washAfter decantation, the chloroform phase is washed with dilute hydrochloric acid
  3. dry with materialwith water, and is dried over anhydrous sodium sulfate
  4. customEvaporation of the solvent
  5. customin vacuo, leaves crystals which
  6. customare recrystallized from methanol

出典と根拠

ORDレコード
ord-56517607782d415fbf62b84c9158e6f3
出典データセット
uspto-grants-1985_01
特許番号
US04496568

反応ノート

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