Triethylamine → HCID 22008838、化合物

HRID 321999ノート

反応式

HRID 321999 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4](Cl)=[O:5].[NH:12]1[CH:17]=[CH:16][C:15](=[O:18])[CH2:14][CH2:13]1.C(N(CC)CC)C>ClCCl.O>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([N:12]1[CH:13]=[CH:14][C:15](=[O:18])[CH2:16][CH2:17]1)=[O:5]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 27568702-Bromo-6-chlorobenzoyl chlorideHCID 122236381,2,3,4-Tetrahydropyridin-4-one

生成物 1

HCID 22008838HCID 22008838、化合物収率 399.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 2-bromo-6-chlorobenzoic acid chloride (0.5 mmol) in dichloromethane (5 ml) was added dropwise to a solution of 2,3-dihydro-4-pyridinone (5.1 mmol, 495 mg) and triethylamine (1.2 ml) in dichloromethane (20 ml). After stirring for 30 minutes, the solution was diluted with water, separated, the aqueous extract further extracted with dichloromethane, the combined organic extracts combined and washed with brine, dried over sodium sulphate and evaporated. The residue was purified by flash column chromatography on silica eluting with 30% ethyl acetate in hexane to yield the title compound as a pale yellow oil (629 mg). MS (+CI) m/z 316 [M+H]+.

後処理

  1. customseparated
  2. extractionthe aqueous extract further
  3. extractionextracted with dichloromethane
  4. washwashed with brine
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. customThe residue was purified by flash column chromatography on silica eluting with 30% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-08452571f6424a47b7d3c244bd81b0d1
出典データセット
uspto-grants-2001_04
特許番号
US06211189B1

反応ノート

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