4-Bromophenol → HCID 19034153, 화합물

HRID 265911

반응식

HRID 265911 반응식
[C:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15]I)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[Br:17][C:18]1[CH:23]=[CH:22][C:21]([OH:24])=[CH:20][CH:19]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.C(OCC)(=O)C>[Br:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:15][CH2:14][CH:11]2[CH2:12][CH2:13][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH2:9][CH2:10]2)=[CH:20][CH:19]=1

참가 물질

6

반응물 3

HCID 78084-BromophenolHCID 10796Cesium carbonateHCID 9974426Tert-butyl 4-(2-iodoethyl)piperidine-1-carboxylate

생성물 1

HCID 19034153HCID 19034153, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-4 (6.45 g, 19.0 mmol), 4-bromophenol (3.29 g, 19 mmol), and Cs2CO3 (3.10 g, 9.5 mmol) in 50 mL of DMF was stirred at room temperature for 18 hr. The solution was then diluted with 200 mL ethyl acetate and washed with H2O (4×100 mL), then dried over Na2SO4, filtered and concentrated. Flash chromatography (silica, 30% EtOAc/hexanes) gave 36-1 as a white solid.

후처리

  1. washwashed with H2O (4×100 mL)
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3ed9629fbfb44485b5a96afdfa3e2a03
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648368

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