反応式
[Cl:1][C:2]1[C:3]([C:8]([OH:10])=O)=[N:4][CH:5]=[CH:6][CH:7]=1.S(Cl)([Cl:13])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:3]([C:8]([Cl:13])=[O:10])=[N:4][CH:5]=[CH:6][CH:7]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
To a suspension of 3-chloropicolinic acid (1.58 g, 10 mmol) in toluene (6 mL) was added an excess of thionyl chloride (9.52 g, 5.84 mL, 80.0 mmol) at room temperature under a nitrogen atmosphere. The resulting suspension was heated to 120° C. (oil bath temperature) and stirred for 20 h. Then, the solvent and excess of thionyl chloride were removed under vacuum and the residue was dissolved one more time in toluene and the solvent was removed again. The resulting residue was dried under high vacuum and used in the next step.
後処理
- customThen, the solvent and excess of thionyl chloride were removed under vacuum
- dissolutionthe residue was dissolved one more time in toluene
- customthe solvent was removed again
- customThe resulting residue was dried under high vacuum
出典と根拠
- ORDレコード
- ord-0c111a772a66422795d657a647f2ebe2
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09199987B2
関連ノート
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