Oxonium, triethyl-, hexafluorophosphate(1-) (1:1) → ethyl (2S)-1-[(4-fluorophenyl)sulfonyl]-2-piperidinecarboximidate

HRID 397665노트

반응식

HRID 397665 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C@H:12]2[C:17]([NH2:19])=[O:18])(=[O:10])=[O:9])=[CH:4][CH:3]=1.F[P-](F)(F)(F)(F)F.[CH2:27]([O+](CC)CC)[CH3:28]>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C@H:12]2[C:17](=[NH:19])[O:18][CH2:27][CH3:28])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 167684Oxonium, triethyl-, hexafluorophosphate(1-) (1:1)HCID 8402010(2S)-1-[(4-Fluorophenyl)sulfonyl]-2-piperidinecarboxamide

생성물 1

HCID 57097015ethyl (2S)-1-[(4-fluorophenyl)sulfonyl]-2-piperidinecarboximidate수율 92.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

(2S)-1-[(4-Fluorophenyl)sulfonyl]-2-piperidinecarboxamide (286 mg) [see Preparation 40] was added to a solution of triethyloxonium hexafluorophosphate (304 mg) in dichloromethane (5 ml). The reaction mixture was stirred at room temperature for 18 hours after which time the mixture was diluted with dichloromethane and washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was separated, dried over magnesium sulphate and the solvent was removed under reduced pressure to afford ethyl (2S)-1-[(4-fluorophenyl)sulfonyl]-2-piperidinecarboximidate (290 mg).

후처리

  1. washwashed with saturated aqueous sodium hydrogen carbonate solution
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulphate
  4. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-d61357ce9d34439fa98d3b9052b5191a
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610707B1

반응 노트

불러오는 중…