Water → 2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde

HRID 840374ノート

反応式

HRID 840374 の反応式
C([O:3][C:4](=O)[CH:5]([O:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]2OCC[O:15]2)=[CH:10][C:9]=1[N+:19]([O-])=O)[CH3:6])C.O>C(O)(=O)C.[Fe]>[CH:14]([C:11]1[CH:12]=[CH:13][C:8]2[O:7][CH:5]([CH3:6])[C:4](=[O:3])[NH:19][C:9]=2[CH:10]=1)=[O:15]

参加物

5

反応物 2

HCID 962Water2 回HCID 57232269HCID 57232269、化合物

生成物 1

HCID 218738872-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde収率 97.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

28.8 g of pulverized iron is added in portions to 34 g of 2-(4-(1,3-dioxolan-2-yl)-2-nitrophenoxy)propionic acid ethyl ester in 360 ml of glacial acetic acid with 80 ml of water while being cooled in an ice bath. The mixture is hot. After 2 hours, it is poured onto 1 l of water, extracted with ethyl acetate, and the organic phase is washed with brine. It is dried with magnesium sulfate and concentrated by evaporation. 20.3 g of brownish solid results.

後処理

  1. temperaturewhile being cooled in an ice bath
  2. extractionextracted with ethyl acetate
  3. washthe organic phase is washed with brine
  4. dry with materialIt is dried with magnesium sulfate
  5. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-ed45fd133e4c4bba840060cc69578bfd
出典データセット
uspto-grants-2002_04
特許番号
US06365736B1

反応ノート

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