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Sodium Hydroxide → 4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-1,2-thiazol-3-yl]-N-[(E)-ethoxyiminomethyl]-2-methylbenzamide

HRID 1522783
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HRID 1522783 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:24]([F:27])([F:26])[F:25])[S:13][N:12]=[C:11]([C:14]3[CH:22]=[CH:21][C:17]([C:18]([NH2:20])=[O:19])=[C:16]([CH3:23])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[CH3:28]OC(OC)N(C)C.Cl.[CH2:37]([O:39][NH2:40])[CH3:38].[OH-].[Na+]>O.C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:24]([F:25])([F:27])[F:26])[S:13][N:12]=[C:11]([C:14]3[CH:22]=[CH:21][C:17]([C:18]([NH:20]/[CH:28]=[N:40]/[O:39][CH2:37][CH3:38])=[O:19])=[C:16]([CH3:23])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 76850O-ethylhydroxylamine hydrochlorideHCID 78373Dimethylformamide dimethyl acetalHCID 894445764-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-isothiazol-3-yl]-2-methyl-benzamide

생성물 1

HCID 1365993674-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-1,2-thiazol-3-yl]-N-[(E)-ethoxyiminomethyl]-2-methylbenzamide

시약·촉매·용매

2
HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A solution of 4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-isothiazol-3-yl]-2-methyl-benzamide (200 mg) and N,N-Dimethylformamide dimethylacetal (4 mL) was refluxed under Argon for one hour then the solution was concentrated in vacuo. The residue was dissolved in 1,4-dioxane (2 mL) and a solution of O-ethylhydroxylamine hydrochloride (2.8 eq.) and sodium hydroxide (6 eq.) in water (1.6 mL) and acetic acid (1.6 mL) was added. The solution was stirred at rt for 10 minutes. It was then quenched by addition of water and extracted with methyl tert-butyl ether. The combined organic extracts were washed with brine, dried over magnesium sulfate and evaporated. Flash Chromatography eluting with Cyclohexane:EtOAc afforded 237 mg of the title compound.

후처리

  1. concentrationthe solution was concentrated in vacuo
  2. dissolutionThe residue was dissolved in 1,4-dioxane (2 mL)
  3. customIt was then quenched by addition of water
  4. extractionextracted with methyl tert-butyl ether
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. washFlash Chromatography eluting with Cyclohexane

출처 및 근거

ORD 기록
ord-aae3819e03b24a4191bbd934034b74f8
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09078444B2

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