Potassium Iodide → Phosphoric Acid di-tert-butyl Ester 2,5-dioxo-4,4-diphenyl-imidazolidin-1-ylmethyl Ester

HRID 377025

반응식

HRID 377025 반응식
Cl[CH2:2][N:3]1[C:7](=[O:8])[C:6]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:5][C:4]1=[O:21].[P:22]([O-:34])([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23].[K+].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(#N)C>[O:21]=[C:4]1[NH:5][C:6]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:8])[N:3]1[CH2:2][O:34][P:22](=[O:23])([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])[O:29][C:30]([CH3:31])([CH3:32])[CH3:33]

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 110986333-(Chloromethyl)-5,5-diphenylimidazolidine-2,4-dioneHCID 23674467Potassium di-tert-butyl phosphate

생성물 1

HCID 15459545Phosphoric Acid di-tert-butyl Ester 2,5-dioxo-4,4-diphenyl-imidazolidin-1-ylmethyl Ester수율 38.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
0 °C

실험 절차

35.5 Grams of 3-(chloromethyl)-5,5-diphenyl-2,4-imidazolidinedione from Step (A), 30.7 g of potassium di(t-butyl) phosphate, 0.6 g of potassium carbonate, and 0.15 g of potassium iodide were slurried into 200 mL acetonitrile. The reaction mixture was heated at reflux for 2.5 hours. The solution was filtered to remove potassium chloride precipitate. The filtrate was cooled to 0° C. and filtered to give 22.3 g of the title compound (38.6% yield); mp 108.5° C. (d). 1H NMR (DMSO-d6): 1.3 ppm (s, 18H), 5.2 (d, 2H), 7.3-7.5 (m, 10H), 9.9 (s, 1H); doublet from long range phosphorus coupling.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 2.5 hours
  3. filtrationThe solution was filtered
  4. customto remove potassium chloride precipitate
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-f7bcfff19c1a4986ad40630688605a06
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022975

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