Piperidine → HCID 43227153, 화합물

HRID 632726

반응식

HRID 632726 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[CH:6]=1)=[O:4].[NH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.CCN(C(C)C)C(C)C>C(Cl)(Cl)Cl>[F:11][C:7]1[CH:6]=[C:5]([C:3](=[O:4])[CH2:2][N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)[CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 81531DiisopropylethylamineHCID 27374513-Fluorophenacyl bromide

생성물 1

HCID 43227153HCID 43227153, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 2-bromo-1-(3-fluoro-phenyl)-ethanone (5.0 g; 23.04 mmol; 1.0 eq.), piperidine (2.30 ml; 23.04 mmol; 1.0 eq.) and DIEA (4.89 ml; 27.65 mmol; 1.20 eq.) in CHCl3 (100 mL) was heated for reflux overnight. The mixture was partitioned between CHCl3 and saturated aqueous NaHCO3. The separated organic layer was dried over MgSO4, filtered and concentrated. The residue was purified through flash chromatography on silica gel to afford the title compound. LC-MS: 222 (M+H).

후처리

  1. temperaturewas heated
  2. temperaturefor reflux overnight
  3. customThe mixture was partitioned between CHCl3 and saturated aqueous NaHCO3
  4. dry with materialThe separated organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified through flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-2da19c8413074eaa81c75190146f05c6
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321760B2

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