Methanol → Methyl 2-chloro-4-thiazolecarboxylate
反応式
S(Cl)(Cl)=O.[Cl:5][C:6]1[S:7][CH:8]=[C:9]([C:11]([OH:13])=[O:12])[N:10]=1.[CH3:14]O>>[Cl:5][C:6]1[S:7][CH:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=1参加物
4
実験手順
Thionyl chloride (4.4 mL, 61 mmol) was added dropwise to a solution of 2-chlorothiazole-4-carboxylic acid (2.00 g, 12.2 mmol) in MeOH (40 mL) at 0° C., and the reaction mixture was allowed to warm to rt. After stirring overnight, the reaction mixture was concentrated under reduced pressure. The resulting solid was recrystallized from EtOH/H2O (1:1), yielding 1.40 g (65%) of the title compound as an orange solid. LC-MS: RT=6.17 min, [M+H]+; =178.1.
後処理
- concentrationthe reaction mixture was concentrated under reduced pressure
- customThe resulting solid was recrystallized from EtOH/H2O (1:1)
出典と根拠
- ORDレコード
- ord-f13948313b6b40f2bf5200d093cd56b2
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09428522B2
反応ノート
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