Dioxoimidazolidine-3-acetate → 5-Hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid

HRID 1416398노트

반응식

HRID 1416398 반응식
[O:1]=C1CNC(=O)N1CC([O-])=O.[N+:12]([C:15]1[CH:16]=[C:17]([CH:31]=[CH:32][CH:33]=1)[CH2:18][N:19]1[C:23](=[O:24])[C:22](=[O:25])[N:21]([CH2:26][C:27]([OH:29])=[O:28])[C:20]1=S)([O-:14])=[O:13]>Cl.O1CCOCC1>[OH:24][CH:23]1[N:19]([CH2:18][C:17]2[CH:31]=[CH:32][CH:33]=[C:15]([N+:12]([O-:14])=[O:13])[CH:16]=2)[C:20](=[O:1])[N:21]([CH2:26][C:27]([OH:29])=[O:28])[C:22]1=[O:25]

참가 물질

5

반응물 2

HCID 2512551Dioxoimidazolidine-3-acetateHCID 106396263-(3-Nitrobenzyl)-4,5-dioxo-2-thioxoimidazolidine-1-acetic acid

생성물 1

HCID 108523655-Hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

The above-prepared dioxoimidazolidine-3-acetate product of paragraph (2) (3.6 g) was dissolved in a mixed solvent of 4N hydrochloric acid and dioxane and the solution was stirred at room temperature for six hours. The reaction solution was concentrated in vacuo to dryness and then chloroform was added to the residue. The crystals were dislodged from the wall of the reaction flask with a spatula. The solid was collected by filtration, washed with chloroform and dried to give 0.8 g of 5-hydroxy-1-(3-nitrobenzyl)-2,4-dioxoimidazolidine-3-acetic acid [Compound 14] as amorphous crystals. The melting point, MS, IR, NMR, and elementary analysis for the compound were:

후처리

  1. concentrationThe reaction solution was concentrated in vacuo to dryness
  2. additionchloroform was added to the residue
  3. filtrationThe solid was collected by filtration
  4. washwashed with chloroform
  5. customdried

출처 및 근거

ORD 기록
ord-d44e976853a54eb69ddafa30fea329b5
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912261

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