Sodium → 7,9-Dioxo-6-aza-spiro[3.5]nonane-8-carboxylic acid methyl ester

HRID 1175168ノート

反応式

HRID 1175168 の反応式
C(O[C:4]([C:6]1([CH2:10][NH:11][C:12](=[O:18])[CH2:13][C:14]([O:16][CH3:17])=[O:15])[CH2:9][CH2:8][CH2:7]1)=[O:5])C.[Na]>C1(C)C=CC=CC=1.CO>[CH3:17][O:16][C:14]([CH:13]1[C:4](=[O:5])[C:6]2([CH2:7][CH2:8][CH2:9]2)[CH2:10][NH:11][C:12]1=[O:18])=[O:15]

参加物

5

反応物 2

HCID 5360545SodiumHCID 57654660HCID 57654660、化合物

生成物 1

HCID 595585517,9-Dioxo-6-aza-spiro[3.5]nonane-8-carboxylic acid methyl ester

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒

実験手順

1-[(2-Methoxycarbonyl-acetylamino)-methyl]-cyclobutanecarboxylic acid ethyl ester (1.62 g, 6.3 mmol) dissolved in 15 ml toluene is added dropwise to a freshly prepared solution of sodium (0.15 g, 6.5 mmol) in methanol (20 ml). The reaction mixture is refluxed for 3 hours and then extracted 3 times with water. The aqueous phase is acidified using HClconc. and the now acidic solution is extracted with ethyl acetate. Drying and evaporation of the solvent delivered the crude product which is used in the next step without further purification.

後処理

  1. temperatureThe reaction mixture is refluxed for 3 hours
  2. extractionextracted 3 times with water
  3. extractionand the now acidic solution is extracted with ethyl acetate
  4. customDrying
  5. customevaporation of the solvent
  6. customis used in the next step without further purification

出典と根拠

ORDレコード
ord-b82e4be28bce4a3585011ce0074a7585
出典データセット
uspto-grants-2010_11
特許番号
US07838674B2

反応ノート

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