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Hydrochloric Acid → 2-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid

HRID 1776989
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인쇄 미리보기

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HRID 1776989 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2([C:29]([F:32])([F:31])[F:30])[CH2:14][CH2:13][N:12]([C:15]3[S:16][C:17]([C:24]([O:26]CC)=[O:25])=[C:18]([C:20]([F:23])([F:22])[F:21])[N:19]=3)[CH2:11]2)[CH:5]=[C:6]([Cl:9])[C:7]=1[Cl:8].[OH-].[Na+].Cl>O1CCOCC1>[Cl:9][C:6]1[CH:5]=[C:4]([C:10]2([C:29]([F:32])([F:30])[F:31])[CH2:14][CH2:13][N:12]([C:15]3[S:16][C:17]([C:24]([OH:26])=[O:25])=[C:18]([C:20]([F:23])([F:21])[F:22])[N:19]=3)[CH2:11]2)[CH:3]=[C:2]([Cl:1])[C:7]=1[Cl:8]
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5

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HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59453365Ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoro-methyl)pyrrolidin-1-yl]-4-(trifluoromethyl)-1,3-thiazole-5-carboxylate

생성물 1

HCID 594533662-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid수율 99%

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

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온도
80 °C

실험 절차

Ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-4-(tri-fluoromethyl)-1,3-thiazole-5-carboxylate (2.4 g) was added to a mixture solution comprising 1,4-dioxane (40 mL) and an aqueous solution (40 mL) of sodium hydroxide (2.0 g), followed by heating at 80° C. for ten hours. After cooling, the reaction solution was poured over ice water, acidified by adding concentrated hydrochloric acid, and then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. The solvent was evaporated off under reduced pressure to obtain the title compound (2.25 g, 99%).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. customThe solvent was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-0e2b92c4653944baa42312750c661154
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266830B2

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