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2-(Methylamino)acetaldehyde → 2-[1-Methyl-3-(5-bromothiazol-2-yl)ureido]acetaldehyde

HRID 839801
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HRID 839801 반응식
[Br:1][C:2]1[S:6][C:5]([N:7]=[C:8]=[O:9])=[N:4][CH:3]=1.[CH3:10][NH:11][CH2:12][CH:13]=[O:14]>C1C=CC=CC=1>[CH3:10][N:11]([CH2:12][CH:13]=[O:14])[C:8]([NH:7][C:5]1[S:6][C:2]([Br:1])=[CH:3][N:4]=1)=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 133161322-(Methylamino)acetaldehydeHCID 230622645-Bromothiazol-2-yl Isocyanate

생성물 1

HCID 227668622-[1-Methyl-3-(5-bromothiazol-2-yl)ureido]acetaldehyde

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

5-Bromothiazol-2-yl isocyanate dimer (17.0 grams), benzene (70 ml) and the dimethyl acetal of 2-methylaminoacetaldehyde (13.5 grams) were charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The reaction mixture was then stirred at room temperature for a period of about one hour. After this time the reaction mixture was filtered, and the filtrate was stripped of solvent under reduced pressure, leaving an oil. This oil was chromatographed on silica gel using ethyl acetate as the diluant. The eluant was dissolved in an ethanol-water mixture, and the solution was filtered. The filtrate was then stripped of solvents under vacuum to yield the desired product the dimethyl acetal of 2-[1-methyl-3-(5-bromothiazol-2-yl)ureido]acetaldehyde as a crystalline solid having a melt point of 72° to 73° C.

후처리

  1. customequipped with a mechanical stirrer
  2. filtrationAfter this time the reaction mixture was filtered
  3. customleaving an oil
  4. customThis oil was chromatographed on silica gel
  5. dissolutionThe eluant was dissolved in an ethanol-water mixture
  6. filtrationthe solution was filtered

출처 및 근거

ORD 기록
ord-b0496a1df3f64592a778f5741f5a8530
출처 데이터셋
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04097485

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