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Ethanol → Tert-butyl 2,4-dioxo-1,3,7-triazaspiro[4.5]decane-7-carboxylate

HRID 1639995
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인쇄 미리보기

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HRID 1639995 반응식
O=[C:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:3]1.[C-]#N.[K+].[C:18](=[O:21])([O-])[O-].[NH4+:22].[NH4+:23].[CH2:24]([OH:26])C>O.C(OCC)(=O)C>[O:26]=[C:24]1[NH:23][C:18](=[O:21])[C:2]2([CH2:7][CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:3]2)[NH:22]1
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참가 물질

7

반응물 4

HCID 702EthanolHCID 9032Potassium CyanideHCID 517111Ammonium CarbonateHCID 2756825Tert-butyl 3-oxopiperidine-1-carboxylate

생성물 1

HCID 42614218Tert-butyl 2,4-dioxo-1,3,7-triazaspiro[4.5]decane-7-carboxylate

시약·촉매·용매 2

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

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온도
70 °C

실험 절차

A mixture of tert-butyl 3-oxopiperidine-1-carboxylate (0.20 g, 0.0010 mol), potassium cyanide (0.13 g, 0.0020 mol) and ammonium carbonate (0.77 g, 0.0080 mol) in ethanol (4.0 mL, 0.068 mol) and water (2.0 mL) was stirred at 70° C. for 4 h. The mixture was then diluted with ethyl acetate and washed with water, brine, dried and concentrated to give the desired product. LC-MS: 292.0 (M+Na)+.

후처리

  1. washwashed with water, brine
  2. customdried
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-270b8f78de4545c7a1aad7ad8712852a
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08110581B2

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