Methyl morpholine oxide → 2-Methyl-5-nitro-4-oxo-4H-1-benzopyran-8-carbaldehyde

HRID 557427ノート

反応式

HRID 557427 の反応式
Br[CH:2](Br)[C:3]1[CH:4]=[CH:5][C:6]([N+:15]([O-:17])=[O:16])=[C:7]2[C:12]=1[O:11][C:10]([CH3:13])=[CH:9][C:8]2=[O:14].C[N+]1([O-])CC[O:23]CC1>C(#N)C>[CH3:13][C:10]1[O:11][C:12]2[C:7]([C:8](=[O:14])[CH:9]=1)=[C:6]([N+:15]([O-:17])=[O:16])[CH:5]=[CH:4][C:3]=2[CH:2]=[O:23]

参加物

4

反応物 2

HCID 82029Methyl morpholine oxideHCID 578286378-(Dibromomethyl)-2-methyl-5-nitro-4H-1-benzopyran-4-one

生成物 1

HCID 578286522-Methyl-5-nitro-4-oxo-4H-1-benzopyran-8-carbaldehyde

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

175 mg (0.47 mmol) of 8-(dibromomethyl)-2-methyl-5-nitro-4H-chromen-4-one are heated under reflux with 151 mg (1.29 mmol) of N-methylmorpholine N-oxide with the addition of molecular sieves in 15 ml of acetonitrile overnight. After filtration through kieselguhr, the solvent is removed in vacuo, and the residue is purified by preparative HPLC. 23 mg (24% of theory) of the title compound are obtained.

後処理

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

出典と根拠

ORDレコード
ord-94997dea25a14cd89bbdf53f3e0bc59d
出典データセット
uspto-grants-2011_11
特許番号
US08058447B2

反応ノート

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