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Methyl formate → HCID 13337060, 화합물

HRID 484637
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HRID 484637 반응식
[C:1]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N:9]=[C:10]1[N:15]([CH3:16])[C:14](=[O:17])[N:13]([CH3:18])[C:12](=[O:19])[C:11]1=[N:20]O)([OH:3])=[O:2].[CH:22](OC)=[O:23]>[Pt]=O.CO>[C:1]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][NH:9][C:10]1[N:15]([CH3:16])[C:14](=[O:17])[N:13]([CH3:18])[C:12](=[O:19])[C:11]=1[NH:20][CH:22]=[O:23])([OH:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 7865Methyl formateHCID 178481575HCID 178481575, 화합물

생성물 1

HCID 13337060HCID 13337060, 화합물수율 63%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 887Methanol용매

실험 절차

A mixture of 15.8 g (0.05 mol) of the oxime (III), 200 ml of methanol, and 100 mg of platinum oxide was shaken under 4 atmospheres H2 for 15 minutes at room temperature. The catalyst was removed by filtration and the filtrate concentrated under reduced pressure (35° C.) to give a red oil. Methyl formate (200 ml) was added and the resulting mixture refluxed under argon for 20 hours. It was then cooled in an ice bath and the white solid collected by filtration. Recrystallization from methanol gave 9.82 g (63% yield) of the formamido uracil (IV) as white crystals, mp 152°-153° C.

후처리

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate concentrated under reduced pressure (35° C.)
  3. customto give a red oil
  4. temperaturethe resulting mixture refluxed under argon for 20 hours
  5. temperatureIt was then cooled in an ice bath
  6. filtrationthe white solid collected by filtration
  7. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-9f1a9d564f0c4ab3b6397b7b954cbe9e
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04533493

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