Triethylamine → HCID 22008838, 화합물

HRID 321999노트

반응식

HRID 321999 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 22008838HCID 22008838, 화합물수율 399.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-08452571f6424a47b7d3c244bd81b0d1
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211189B1

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