Phosphorus oxychloride → 2-Chloro-5-isopropylpyrimidine
反応式
[CH:1]([C:4]1[CH:5]=[N:6][C:7](=O)[NH:8][CH:9]=1)([CH3:3])[CH3:2].O=P(Cl)(Cl)[Cl:13]>CN(C)C1C=CC=CC=1>[Cl:13][C:7]1[N:6]=[CH:5][C:4]([CH:1]([CH3:3])[CH3:2])=[CH:9][N:8]=1参加物
4
実験手順
A mixture of 5-isopropylpyrimidin-2(1H)-one (2.1 g, 15.2 mmol), POCl3 (15 ml), and N,N-dimethylaniline (5 drops) was heated at reflux under a nitrogen atmosphere for 2 h. Upon cooling, the majority of the POCl3 was removed under reduced pressure. The residue was poured into ice water and extracted with chloroform (3×20 ml). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated to provide 2-chloro-5-isopropylpyrimidine as a light brown oil, which was used without further purification.
後処理
- temperaturewas heated
- temperatureat reflux under a nitrogen atmosphere for 2 h
- temperatureUpon cooling
- customthe majority of the POCl3 was removed under reduced pressure
- additionThe residue was poured into ice water
- extractionextracted with chloroform (3×20 ml)
- washThe combined organic extracts were washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-fb309df154684408a961ba21676f4e49
- 出典データセット
- uspto-grants-2008_01
- 特許番号
- US07319104B2
反応ノート
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