Potassium Iodide → HCID 23081539, 화합물

HRID 856281노트

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HRID 856281 반응식
CS(O[CH2:6][CH2:7][CH2:8][C:9]1([CH3:20])[O:13][C:12]2=[N:14][C:15]([N+:17]([O-:19])=[O:18])=[CH:16][N:11]2[CH2:10]1)(=O)=O.[N:21]1([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(N(CC)CC)C.[I-].[K+]>CN(C=O)C>[CH3:20][C:9]1([CH2:8][CH2:7][CH2:6][N:24]2[CH2:23][CH2:22][N:21]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:26][CH2:25]2)[O:13][C:12]2=[N:14][C:15]([N+:17]([O-:19])=[O:18])=[CH:16][N:11]2[CH2:10]1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 23081120HCID 23081120, 화합물

생성물 1

HCID 23081539HCID 23081539, 화합물수율 73%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A mixture of 3-(2-methyl-6-nitro-2,3-dihydroimidazo[2,1-b]oxazol-2-yl)propyl methane-sulfonate (2 g, 6.6 mmol), tert-butyl piperazine-1-carboxylate (1.4 g, 7.5 mmol), triethylamine (1.3 g, 12.85 mmol), potassium iodide (1.8 g, 10.8 mmol) and DMF (15 ml) was stirred at 60° C. overnight. The reaction mixture was allowed to return to room temperature and then added water, and the resulting solution was extracted with ethyl acetate three times. The organic phases were combined, washed with water twice and then with a saturated saline solution, dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/methanol=20/1) to afford tert-butyl 4-[3-(2-methyl-6-nitro-2,3-dihydroimidazo[2,1-b]oxazol-2-yl)propyl]piperazine-1-carboxylate (1.9 g, yield 73%) as a white powder.

후처리

  1. customto return to room temperature
  2. extractionadded water, and the resulting solution was extracted with ethyl acetate three times
  3. washwashed with water twice
  4. dry with materialwith a saturated saline solution, dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=20/1)

출처 및 근거

ORD 기록
ord-bb8de93a08e346ec8cbdcf1a695f6c8d
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262212B2

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