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

HRID 1175168노트

반응식

HRID 1175168 반응식
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]

참가 물질

5

반응물 2

HCID 5360545SodiumHCID 57654660HCID 57654660, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b82e4be28bce4a3585011ce0074a7585
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838674B2

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