Methyl morpholine oxide → 5-Chloro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde

HRID 1669778ノート

反応式

HRID 1669778 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([CH:12](Br)Br)=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([CH3:15])[O:7]2.C[N+]1([O-])CC[O:21]CC1>C(#N)C>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([CH:12]=[O:21])=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([CH3:15])[O:7]2

参加物

4

反応物 2

HCID 82029Methyl morpholine oxideHCID 574388935-chloro-8-(dibromomethyl)-2-methyl-4H-chromen-4-one

生成物 1

HCID 574388945-Chloro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

210 mg (0.57 mmol) of 5-chloro-8-(dibromomethyl)-2-methyl-4H-chromen-4-one are heated with 147 mg (1.2 mmol) of N-methylmorpholine N-oxide with the addition of molecular sieves in 15 ml of acetonitrile under reflux overnight. After filtration through kieselguhr, the solvent is removed in vacuo and the residue is purified by preparative HPLC. 22 mg (17% of theory) of the title compound are obtained.

後処理

  1. temperatureunder reflux overnight
  2. filtrationAfter filtration through kieselguhr
  3. customthe solvent is removed in vacuo
  4. customthe residue is purified by preparative HPLC

出典と根拠

ORDレコード
ord-61f0625179394896a07f395e4e343a5d
出典データセット
uspto-grants-2011_08
特許番号
US07989633B2

反応ノート

読み込み中…