Piperidine → HCID 43227153、化合物

HRID 632726ノート

反応式

HRID 632726 の反応式
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

参加物

5

反応物 3

HCID 8082PiperidineHCID 81531DiisopropylethylamineHCID 27374513-Fluorophenacyl bromide

生成物 1

HCID 43227153HCID 43227153、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2da19c8413074eaa81c75190146f05c6
出典データセット
uspto-grants-2016_04
特許番号
US09321760B2

反応ノート

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