Phosphorus oxychloride → Ethyl 6-chloro-1,2,4-triazine-5-carboxylate

HRID 2076829노트

반응식

HRID 2076829 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:11](=O)[NH:10][N:9]=[CH:8][N:7]=1)=[O:5])[CH3:2].O=P(Cl)(Cl)[Cl:15]>>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]=[N:10][C:11]=1[Cl:15])=[O:5])[CH3:2]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 117152386-Oxo-1,6-dihydro-[1,2,4]triazine-5-carboxylic acid ethyl ester

생성물 1

HCID 72213151Ethyl 6-chloro-1,2,4-triazine-5-carboxylate수율 90%

실험 절차

6-Oxo-1,6-dihydro-[1,2,4]triazine-5-carboxylic acid ethyl ester (115 mg, 0.68 mmol) in POCl3 (1.5 ml) was heated to 100° C. for 2 h. All volatiles were then removed and the remaining residue was diluted with cold CHCl3 and carefully neutralized with sat. NaHCO3-solution. This mixture was extracted with cold CHCl3. The organic phase was then washed with cold brine, dried (Na2SO4) and evaporated to give the crude title compound (115 mg, 90%) as brown gum, which was used in the next reaction step without further purification. MS: m/e=188.2 [M+H+].

후처리

  1. customAll volatiles were then removed
  2. additionthe remaining residue was diluted with cold CHCl3
  3. extractionThis mixture was extracted with cold CHCl3
  4. washThe organic phase was then washed with cold brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-68918494679341918845bb9785d0d5fb
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928106B2

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