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

HRID 1179849

反応式

HRID 1179849 の反応式
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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 109478841-methyl-3-(methyl-phenyl-carbamoyl)-3H-imidazol-1-ium iodideHCID 178479648HCID 178479648、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8a5a87f3c6b84e28a0b70b95bc49243a
出典データセット
uspto-grants-2007_10
特許番号
US07279470B2

関連ノート

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