3-Methyl-2,4-pentanedione → HCID 178424484, 화합물

HRID 1813923노트

반응식

HRID 1813923 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH2:16].C[CH:18]([C:22](=O)[CH3:23])[C:19](=[O:21])C>>[CH3:23][C:22]1[CH:18]=[C:19]([OH:21])[C:12]2[C:11](=[C:10]([C:3]3[C:4]([CH3:9])=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=3[CH3:1])[CH:15]=[CH:14][CH:13]=2)[N:16]=1

참가 물질

3

반응물 2

HCID 699493-Methyl-2,4-pentanedioneHCID 137578442-(2,4,6-Trimethylphenyl)aniline

생성물 1

HCID 178424484HCID 178424484, 화합물

반응 조건

온도
170 °C

실험 절차

A mixture of 2′,4′,6′-trimethyl-biphenyl-2-ylamine(607 mg, 2.88 mmol) and methyl acetylacetone (607 mg, 5.75 mmol) in polyphosphoric acid (3 ml) was heated in 170° C. oil bath for 2.5 hours. The mixture was quenched with water and extracted twice with chloroform. The organic layer was washed with brine, dried and concentrated to give the title compound as an oil. The oil was pumped in vacuo, then trituated with a mixture of ether and hexane to give 642 mg (81%) of the title compound as a beige solid. The solid was recrystallized from ethyl acetate to give a beige solid, mp>250° C.

후처리

  1. customThe mixture was quenched with water
  2. extractionextracted twice with chloroform
  3. washThe organic layer was washed with brine
  4. customdried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f5babae7267c4e94846f1761de8ceb10
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875769B2

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