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

HRID 840374노트

반응식

HRID 840374 반응식
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]

참가 물질

5

반응물 2

HCID 962Water2회HCID 57232269HCID 57232269, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ed45fd133e4c4bba840060cc69578bfd
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06365736B1

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