홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium hydride → tert-butyl 4-[(E)-2-(2-chloro-6-methylphenyl)vinyl]piperidine-1-carboxylate

HRID 1667308
노트
인쇄 미리보기

반응식

HRID 1667308 반응식
[H-].[Na+].[Cl-].[Cl:4][C:5]1[CH:30]=[CH:29][CH:28]=[C:27]([CH3:31])[C:6]=1[CH2:7][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH:32]([CH:34]1[CH2:39][CH2:38][N:37]([C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41])[CH2:36][CH2:35]1)=O.[Cl-].[NH4+]>CS(C)=O>[Cl:4][C:5]1[CH:30]=[CH:29][CH:28]=[C:27]([CH3:31])[C:6]=1/[CH:7]=[CH:32]/[CH:34]1[CH2:39][CH2:38][N:37]([C:40]([O:42][C:43]([CH3:44])([CH3:46])[CH3:45])=[O:41])[CH2:36][CH2:35]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 1514430tert-Butyl 4-formylpiperidine-1-carboxylateHCID 86612298(2-Chloro-6-methylbenzyl)(triphenyl)phosphonium chloride

생성물 1

HCID 10088346tert-butyl 4-[(E)-2-(2-chloro-6-methylphenyl)vinyl]piperidine-1-carboxylate수율 41.2%

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

실험 절차

264 mg of sodium hydride (55%) was added to a solution of 2.65 g of (2-chloro-6-methylbenzyl)(triphenyl)phosphonium chloride in 20 ml of dimethylsulfoxide, followed by stirring at ambient temperature for 1 hour. After 994 mg of tert-butyl 4-formylpiperidine-1-carboxylate was added to the reaction mixture, the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was poured into saturated aqueous ammonium chloride, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and then dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated and the resulting residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give 645 mg of tert-butyl 4-[(E)-2-(2-chloro-6-methylphenyl)vinyl]piperidine-1-carboxylate as an oil.

후처리

  1. stirringthe mixture was stirred at ambient temperature for 1 hour
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated
  7. customthe resulting residue was purified by silica gel column chromatography (hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-03f1f2baaaac4708b07d89e49e4052f2
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044206B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트