Triethylamine → 4-t-Butylsulfinylamino-1-ethoxycarbonyl piperidine

HRID 1641592

반응식

HRID 1641592 반응식
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]1.C(N(CC)CC)C.[C:20]([S:24](Cl)=[O:25])([CH3:23])([CH3:22])[CH3:21]>ClCCl>[C:20]([S:24]([NH:1][CH:2]1[CH2:3][CH2:4][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:6][CH2:7]1)=[O:25])([CH3:23])([CH3:22])[CH3:21]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 100867Ethyl 4-amino-1-piperidinecarboxylateHCID 46868612-Methylpropane-2-sulfinyl chloride

생성물 1

HCID 227477804-t-Butylsulfinylamino-1-ethoxycarbonyl piperidine수율 86.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Ethyl 4-amino-1-piperidinecarboxylate (300 mg) and triethylamine (258 mg) were dissolved in 5 ml of dichloromethane. To the mixture, 2 ml of solution of t-butylsulfinyl chloride (222 mg) in dichloromethane was added and the mixture was stirred at room temperature for 4 hours. The solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate anhydride. The solvent was removed under reduced pressure and the residue was purified by silica gel chromatography to give 378 mg of 4-t-butylsulfinylamino-1-ethoxycarbonyl piperidine.

후처리

  1. customThe solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate anhydride
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-90bf8fde81d040c9b35eb024cdc57133
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08115027B2

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