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

HRID 2413129노트

반응식

HRID 2413129 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-56517607782d415fbf62b84c9158e6f3
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04496568

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