Hydrochloric Acid → Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic Acid Methyl Ester

HRID 2388658노트

반응식

HRID 2388658 반응식
Cl.[CH3:2][O:3][C:4](=[O:15])[CH:5]([CH3:14])[CH2:6][CH2:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][NH:9]1.C(N(CC)CC)C.[CH3:23][O:24][C:25]1[CH:30]=[C:29]([CH3:31])[C:28]([S:32](Cl)(=[O:34])=[O:33])=[C:27]([CH3:36])[CH:26]=1.Cl>C(Cl)Cl>[CH3:2][O:3][C:4](=[O:15])[CH:5]([CH3:14])[CH2:6][CH2:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][N:9]1[S:32]([C:28]1[C:29]([CH3:31])=[CH:30][C:25]([O:24][CH3:23])=[CH:26][C:27]=1[CH3:36])(=[O:34])=[O:33]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 159174964-Methoxy-2,6-dimethylbenzene-1-sulfonyl chlorideHCID 67316706Methyl 4-(piperidin-2-yl)butanoic acid methyl ester hydrochloride

생성물 1

HCID 67316484Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic Acid Methyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

Methyl 4-(piperidin-2-yl)butanoic acid methyl ester hydrochloride (1.26 g, 5.683 mmol) was dissolved in methylene chloride (25 ml) and triethylamine (4 ml, 28.417 mmol) and a solution of 4-methoxy-2,6-dimethylbenzenesulfonic acid chloride (2.67 g, 11.37 mmol) [see AC5, stage 1) in methylene chloride (10 ml) was added. The mixture was stirred at room temperature overnight. 1 mol/l HCl solution (10 ml) was added to the reaction mixture, phase separation, extraction of the aqueous phase with methylene chloride (2×20 ml). The combined organic phases were washed with sat. sodium chloride solution (20 ml), dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with hexane/methylene chloride/ether (400/100/50). The yield was 1.65 g (75%).

후처리

  1. additionwas added
  2. washThe combined organic phases were washed with sat. sodium chloride solution (20 ml)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by column chromatography (silica gel) with hexane/methylene chloride/ether (400/100/50)

출처 및 근거

ORD 기록
ord-9d8123e5b9e44ff3868408747bf50f03
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268814B2

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