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

Potassium Carbonate → (3S)-tert-butyl 3-(3-hydroxy-5-methyl-3-phenylhex-5-enylamino)piperidine-1-carboxylate

HRID 884352
노트
인쇄 미리보기

반응식

HRID 884352 반응식
Cl[CH2:2][CH2:3][C:4]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([OH:9])[CH2:5][C:6]([CH3:8])=[CH2:7].[NH2:16][C@H:17]1[CH2:22][CH2:21][CH2:20][N:19]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:18]1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[OH:9][C:4]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH2:5][C:6]([CH3:8])=[CH2:7])[CH2:3][CH2:2][NH:16][C@H:17]1[CH2:22][CH2:21][CH2:20][N:19]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1501975tert-butyl (3S)-3-aminopiperidine-1-carboxylateHCID 595323881-Chlor-5-methyl-3-phenylhex-5-en-3-ol

생성물 1

HCID 58278669(3S)-tert-butyl 3-(3-hydroxy-5-methyl-3-phenylhex-5-enylamino)piperidine-1-carboxylate수율 94.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-chloro-5-methyl-3-phenylhex-5-en-3-ol (5.16g, 23mmol), (S)-tert-butyl 3-aminopiperidine-1-carboxylate (6.9 g, 1.5 equiv), KI (4.0 g, 1.05 equiv), K2CO3 (4.77 g, 1.5 equiv) were mixed with acetonitrile (100 mL) and heated to reflux for 20 h. The mixture was filtered through a pad of Celite, concentrated and purified by chromatography on a 120 g silica gel column, eluted with a 0-10% methanol in CH2Cl2 gradient, to afford (3S)-tert-butyl 3-(3-hydroxy-5-methyl-3-phenylhex-5-enylamino)piperidine-1-carboxylate (8.41 g, 94% yield). LC-MS Method 1 tR=1.56 min., m/z 389 (M+1).

후처리

  1. temperatureheated
  2. temperatureto reflux for 20 h
  3. filtrationThe mixture was filtered through a pad of Celite
  4. concentrationconcentrated
  5. custompurified by chromatography on a 120 g silica gel column
  6. washeluted with a 0-10% methanol in CH2Cl2 gradient

출처 및 근거

ORD 기록
ord-38a9be6253544a768da081d8ee396bac
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08242111B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트