Ethanol → 2,8-Diazaspiro[4.5]decane-1,3-dione

HRID 491472노트

반응식

HRID 491472 반응식
C([N:8]1[CH2:19][CH2:18][C:11]2([C:15](=[O:16])[NH:14][C:13](=[O:17])[CH2:12]2)[CH2:10][CH2:9]1)C1C=CC=CC=1.CCO>[OH-].[OH-].[Pd+2].C(O)(=O)C>[C:15]1(=[O:16])[C:11]2([CH2:10][CH2:9][NH:8][CH2:19][CH2:18]2)[CH2:12][C:13](=[O:17])[NH:14]1

참가 물질

5

반응물 2

HCID 702EthanolHCID 221109398-Benzyl-2,8-diazaspiro[4.5]decane-1,3-dione

생성물 1

HCID 156710412,8-Diazaspiro[4.5]decane-1,3-dione

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 176Acetic Acid용매

실험 절차

To 8-benzyl-2,8-diaza-spiro[4.5]decane-1,3-dione (28.3 g, 0.11 mol) and Pd(OH)2 (8.5 g) in 2 l of flask, EtOH (438 ml) and acetic acid (5.5 ml) are added at ambient temperature. The reaction mixture is stirred under H2 at room temperature for 15 h. The catalysts are removed by filtration and EtOH is evaporated down to give 2,8-diaza-spiro[4.5]decane-1,3-dione in quantitative yield. To a suspension of 2,8-diaza-spiro[4.5]decane-1,3-dione (4.2 g, 25.2 mmol) in dichloromethane (60 ml), 1N NaOH (26 ml, 26 mmol) and di-t-butyldicarbonate (6.1 g, 27.7 mmol) in dichloromethane (20 ml) are added at ambient temperature. The reaction mixture is stirred for 15 h. 10% Citric acid is added to the reaction mixture and the pH of the mixture is adjusted to 5. The combined extracts are washed with brine, dried over magnesium sulfate and concentrated under vacuum to give solid product, which filtrated with diethyl ether.

후처리

  1. customThe catalysts are removed by filtration and EtOH
  2. customis evaporated down

출처 및 근거

ORD 기록
ord-6bf8d4cb5fab4e6f8501cf33cdb0a427
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531546B2

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