Triethylamine → Methyl-phenyl-carbamic Acid pyrimidin-2-yl Ester

HRID 1179849

반응식

HRID 1179849 반응식
Cl.[OH:2][C:3]1[N:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[I-].C[N+]1C=CN([C:16](=[O:25])[N:17]([CH3:24])[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)C=1.C(N(CC)CC)C>C(#N)C>[N:4]1[CH:5]=[CH:6][CH:7]=[N:8][C:3]=1[O:2][C:16](=[O:25])[N:17]([CH3:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 109478841-methyl-3-(methyl-phenyl-carbamoyl)-3H-imidazol-1-ium iodideHCID 178479648HCID 178479648, 화합물

생성물 1

HCID 69518913Methyl-phenyl-carbamic Acid pyrimidin-2-yl Ester수율 12%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 2-hydroxypyrimidine hydrochloride (0.40 g, 3.00 mmol), 1-methyl-3-(methyl-phenyl-carbamoyl)-3H-imidazol-1-ium iodide (1.03 g, 3.00 mmol) and triethylamine (0.83 ml, 6.00 mmol) in acetonitrile (15 ml) was stirred at room temperature overnight. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography (SiO2, ethyl acetate) followed by crystallisation from ethyl acetate:heptane yielding the title compound (0.08 g, 12% yield) as a white solid.

후처리

  1. customThe solvent was evaporated in vacuo
  2. customthe residue was purified by flash column chromatography (SiO2, ethyl acetate)
  3. customfollowed by crystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-8a5a87f3c6b84e28a0b70b95bc49243a
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07279470B2

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