Water → Lithium 2-chloro-4-(2,5-dichloro-phenoxy)-6-methyl-nicotinate
Reaction equation
C([O:3][C:4](=[O:22])[C:5]1[C:10]([O:11][C:12]2[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=2[Cl:19])=[CH:9][C:8]([CH3:20])=[N:7][C:6]=1[Cl:21])C.O.O.[OH-].[Li+:26]>O1CCOCC1>[Cl:21][C:6]1[N:7]=[C:8]([CH3:20])[CH:9]=[C:10]([O:11][C:12]2[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=2[Cl:19])[C:5]=1[C:4]([O-:22])=[O:3].[Li+:26]Participants
5
Conditions
- Temperature
- 100 °C
Procedure
To a solution of 130 mg (0.36 mmol) 2-chloro-4-(2,5-dichloro-phenoxy)-6-methyl-nicotinic acid ethyl ester in 2 mL dioxane was added 2 mL water and 23 mg (0.541 mmol) lithium hydroxide monohydrate. The reaction mixture was stirred at 100° C. for 4 hours. The reaction mixture was allowed to cool down to room temperature and was concentrated under high vacuum. The so-obtained light yellow solid was pure enough for the next step without further purification. MS (ESI): 331.965 [M+H]+.
Workup
- temperatureto cool down to room temperature
- concentrationwas concentrated under high vacuum
- customThe so-obtained light yellow solid was pure enough for the next step without further purification
Sources & evidence
- ORD record
- ord-9c34fd8b6b5d4606b19967c909aff8e7
- Source dataset
- uspto-grants-2014_05
- Patent number
- US08729091B2
Reaction notes
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