Pyrrolidine → HCID 58980628、化合物

HRID 735795ノート

反応式

HRID 735795 の反応式
[C:1]([CH:5]([CH:8]=O)[CH:6]=O)([CH3:4])([CH3:3])[CH3:2].[CH3:10][NH:11][C:12](=[O:17])[CH2:13][N+:14]([O-:16])=[O:15].N1CCCC1>C(O)C>[C:1]([C:5]1[CH:6]=[C:13]([N+:14]([O-:16])=[O:15])[C:12](=[O:17])[N:11]([CH3:10])[CH:8]=1)([CH3:2])([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 31268PyrrolidineHCID 574612tert-ButylpropanedialHCID 12512111N-Methylnitroacetamide

生成物 1

HCID 58980628HCID 58980628、化合物収率 30%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-tert-butyl-malonaldehyde (385 mg, 3.00 mmol) and the above amide (355 mg, 3.00 mmol) dissolved in ethanol (6.0 mL) was added pyrrolidine (63 microL, 0.750 mmol). The mixture was heated at reflux for 18 h and concentrated in vacuo. Purification by silica-gel chromatography (75% ethyl acetate in hexanes) provided 5-tert-butyl-1-methyl-3-nitro-1H-pyridin-2-one (186 mg, 30%) as an orange solid.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 18 h
  3. concentrationconcentrated in vacuo
  4. customPurification by silica-gel chromatography (75% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-8d0332f72431433989774f59d4d0a633
出典データセット
uspto-grants-2009_09
特許番号
US07592332B2

反応ノート

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