Sodium Chloride → 1-Methylpiperidin-4-yl methanesulfonate

HRID 1030151노트

반응식

HRID 1030151 반응식
C(N(CC)CC)C.[CH3:8][S:9](Cl)(=[O:11])=[O:10].[OH:13][CH:14]1[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]1.[Cl-].[Na+]>O1CCCC1>[CH3:8][S:9]([O:13][CH:14]1[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]1)(=[O:11])=[O:10]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 660484-Piperidinol, 1-methyl-

생성물 1

HCID 41906811-Methylpiperidin-4-yl methanesulfonate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

13.3 ml of triethylamine and subsequently 7.4 ml of methanesulfonyl chloride were added, whilst ice-cooling, to a solution of 10 g of 4-hydroxy-1-methylpiperidine dissolved in 100 ml of dry tetrahydrofuran. The mixture was then stirred at 0° to 5° C. for 2 hours and then at room temperature for 1.5 hours, after which it was poured into an aqueous solution of sodium chloride and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure, to afford 12.74 g of the title compound as an oil.

후처리

  1. waitat room temperature for 1.5 hours
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with an aqueous solution of sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was then distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-a61438f39f3f4fb09bee510f43af26ad
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104867

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