3-Methyl-2,4-pentanedione → HCID 178424484、化合物

HRID 1813923ノート

反応式

HRID 1813923 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 178424484HCID 178424484、化合物

反応条件

温度
170 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f5babae7267c4e94846f1761de8ceb10
出典データセット
uspto-grants-2005_04
特許番号
US06875769B2

反応ノート

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