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Methanol → N-(2-Methoxy-5-nitrophenyl)-4,4-dimethyl-3-oxopentanamide

HRID 1488905
ノート
印刷プレビュー

反応式

HRID 1488905 の反応式
CO[C:3](=[O:11])[CH2:4][C:5](=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7].[CH3:12][O:13][C:14]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:15]=1[NH2:16].CO>C1(C)C=CC=CC=1>[CH3:9][C:6]([CH3:7])([CH3:8])[C:5](=[O:10])[CH2:4][C:3]([NH:16][C:15]1[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:14]=1[O:13][CH3:12])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 74472-Methoxy-5-nitroanilineHCID 99597Methyl pivaloylacetate

生成物 1

HCID 11162196N-(2-Methoxy-5-nitrophenyl)-4,4-dimethyl-3-oxopentanamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Methyl-4,4-dimethyl-3-oxovalerate (15.8 g, 0.1 mol) and 2-methoxy-5-nitroaniline (16.8 g, 0.01 mol) were taken up in toluene (150 mL) in a round bottomed flask fitted with a Dean-Stark trap. The mixture was heated to a vigorous reflux while the MeOH side-product was distilled off and removed. After 4 hours, the mixture was cooled and the toluene removed in vacuo. The residue was recrystallized from acetonitrile to yield 27 g of the desired condensation product.

後処理

  1. customfitted with a Dean-Stark trap
  2. temperatureThe mixture was heated to
  3. distillationwas distilled off
  4. customremoved
  5. temperaturethe mixture was cooled
  6. customthe toluene removed in vacuo
  7. customThe residue was recrystallized from acetonitrile
  8. customto yield 27 g of the desired
  9. customcondensation product

出典と根拠

ORDレコード
ord-494c3b27ba084c668774250a44afec1e
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05677114

反応ノート

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