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

HRID 1033112

反応式

HRID 1033112 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e171d2619a6f4e12831c6f542031fa3d
出典データセット
uspto-grants-1994_05
特許番号
US05308853

関連ノート

読み込み中…