Butyl iodide → Diethyl 1-Butyl-2,5-Dioxo-4-Imidazolylphosphonate

HRID 1033110

반응식

HRID 1033110 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][CH3:26]>CN(C=O)C.C(OCC)(=O)C>[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][CH3:26]

참가 물질

6

반응물 3

HCID 10962Butyl iodideHCID 11430Potassium CarbonateHCID 53733419Diethyl (2,5-dioxo-2,5-dihydro-1H-imidazol-4-yl)phosphonate

생성물 1

HCID 53922750Diethyl 1-Butyl-2,5-Dioxo-4-Imidazolylphosphonate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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-iodobutane (2.9 mL, 0.025 moles). This mixture is stirred at room temperature for 16 hours and then the mixture is filtered and the solid washed with ethyl acetate. The filtrate is concentrated in vacuo, to afford a yellow oil which is redissolved in ethyl acetate 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 which solidifies on standing.

후처리

  1. filtrationthe mixture is filtered
  2. washthe solid washed with ethyl acetate
  3. concentrationThe filtrate is concentrated in vacuo
  4. customto afford a yellow oil which
  5. washwashed with water and brine
  6. dry with materialdried over MgSO4
  7. customEvaporation of solvents under high vacuum

출처 및 근거

ORD 기록
ord-7a936ccb065a48178c5900250e3ad8ba
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308853

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