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Potassium Hydroxide → Tert-butyl 4-methyl-5-oxoazepane-1-carboxylate

HRID 905969
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인쇄 미리보기

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HRID 905969 반응식
C(O[C:4]([C:6]1(C)[C:12](=[O:13])[CH2:11][CH2:10][N:9]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:8][CH2:7]1)=O)C.[OH-].[K+]>O1CCOCC1>[C:17]([O:16][C:14]([N:9]1[CH2:10][CH2:11][C:12](=[O:13])[CH:6]([CH3:4])[CH2:7][CH2:8]1)=[O:15])([CH3:20])([CH3:18])[CH3:19]
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 67385631HCID 67385631, 화합물

생성물 1

HCID 20594186Tert-butyl 4-methyl-5-oxoazepane-1-carboxylate수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

To a solution of compound 4-methyl-5-oxo-azepane-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester (2.5 g, 8.36 mmol) in dioxane (20 mL) was added 2 M aqueous KOH (20 mL) at 25° C. The resulting solution was stirred at 100° C. for 24 hours before being cooled to RT and extracted twice with EtOAC. The combined organic layers were dried (Na2SO4), filtered, and evaporated to give 1.8 g of 4-methyl-5-oxo-azepane-1-carboxylic acid tert-butyl ester (95% yield).

후처리

  1. temperaturebefore being cooled to RT
  2. extractionextracted twice with EtOAC
  3. dry with materialThe combined organic layers were dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-9aaf8e38448241be8104c0f5260a890f
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08012974B2

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