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Water → Lithium 2-chloro-4-(2,5-dichloro-phenoxy)-6-methyl-nicotinate

HRID 1967054
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HRID 1967054 반응식
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]
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참가 물질

5

반응물 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 866869362-Chloro-4-(2,5-dichloro-phenoxy)-6-methyl-nicotinic acid ethyl ester

생성물 1

HCID 86655954Lithium 2-chloro-4-(2,5-dichloro-phenoxy)-6-methyl-nicotinate

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

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]+.

후처리

  1. temperatureto cool down to room temperature
  2. concentrationwas concentrated under high vacuum
  3. customThe so-obtained light yellow solid was pure enough for the next step without further purification

출처 및 근거

ORD 기록
ord-91120971977b4f2bb032300b2728cb95
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420647B2

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