Potassium Carbonate → HCID 69448964, 화합물

HRID 1593021노트

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HRID 1593021 반응식
[CH2:1]([CH:3]1[NH:7][C:6](=[O:8])[NH:5][C:4]1=[O:9])[CH3:2].C(=O)([O-])[O-].[K+].[K+].CS(O[CH:21]1[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]1)(=O)=O>CN(C=O)C>[CH2:1]([CH:3]1[C:4](=[O:9])[N:5]([CH:21]2[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]2)[C:6](=[O:8])[NH:7]1)[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2532172-EthylhydantoinHCID 41848691-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine

생성물 1

HCID 69448964HCID 69448964, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of 5-ethylimidazoline-2,4-dione (1 g) in DMF (40 ml) was added potassium carbonate (2.16 g) followed by tert-butyl 4-[(methylsulfonyl)oxy]piperidine-1-carboxylate (2.18 g) and the resulting mixture was heated to 100° C. for 18 hours. The reaction mixture was concentrated under reduced pressure and then was partitioned between dichloromethane and water. The organic layer was collected, dried and evaporated to dryness. The residue was purified by chromatography on silica eluting with a gradient of isohexane to ethyl acetate/isohexane (1:1) to give tert-butyl 4(4-ethyl-2,5-dioxoimidazolidin-1-yl)piperidine-1-carboxylate as a solid. Yield 1.12 g. NMR (CDCl3): 0.95 (t, 3H), 1.5 (s, 9H), 1.9 (m, 2H), 2.35 (m, 2H), 2.7 (m, 2H), 3.8-4.0 (m, 3H), 4.1 (q, 2H), 5.6 (bs, 1H).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customwas partitioned between dichloromethane and water
  3. customThe organic layer was collected
  4. customdried
  5. customevaporated to dryness
  6. customThe residue was purified by chromatography on silica eluting with a gradient of isohexane to ethyl acetate/isohexane (1:1)

출처 및 근거

ORD 기록
ord-efe153da3f394f4e9f915650a34ede32
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07294636B2

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