Potassium Carbonate → Diethyl 1-hexyl-2,5-dioxo-4-imidazolylphosphonate

HRID 1033112

반응식

HRID 1033112 반응식
[O:1]=[C:2]1[N:6]=[C:5]([P:7](=[O:14])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])[C:4](=[O:15])[NH:3]1.C([O-])([O-])=O.[K+].[K+].I[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>CN(C=O)C.CCOCC>[CH2:23]([N:3]1[C:4](=[O:15])[C:5]([P:7](=[O:14])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])=[N:6][C:2]1=[O:1])[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 125271-IodohexaneHCID 53733419Diethyl (2,5-dioxo-2,5-dihydro-1H-imidazol-4-yl)phosphonate

생성물 1

HCID 53646860Diethyl 1-hexyl-2,5-dioxo-4-imidazolylphosphonate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of diethyl 2,5-dioxo-4-imidazolylphosphonate (6.00 g, 0.025 moles) in DMF (15 mL), under N2, is added K2CO3 (17.5 g, 0.127 moles) and 1-iodohexane (3.75 mL, 0.025 moles). This mixture is stirred at room temperature for 16 hours. The mixture is diluted with ether (300 mL) and washed with water and brine and then dried over MgSO4. Evaporation of solvents under high vacuum affords the required product as a viscous yellow oil. (Mass spectrometry also revealed a small amount of diethyl 1,3-dihexyl-2,5-dioxo-4-imidazolylphosphonate).

후처리

  1. washwashed with water and brine
  2. dry with materialdried over MgSO4
  3. customEvaporation of solvents under high vacuum

출처 및 근거

ORD 기록
ord-e171d2619a6f4e12831c6f542031fa3d
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308853

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