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Water → 5-Chloro-3-(ethylsulfanyl)-1,2,4-thiadiazole

HRID 1392217
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HRID 1392217 반응식
O.Br.C([NH:5][C:6](=[NH:8])[SH:7])C.[Cl:9][C:10]([SH:13])(Cl)Cl.[OH-].[Na+].[C:16](OC)(C)(C)[CH3:17]>>[CH2:16]([S:7][C:6]1[N:5]=[C:10]([Cl:9])[S:13][N:8]=1)[CH3:17]
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참가 물질

6

반응물 5

HCID 962Water2회HCID 6390TrichloromethanethiolHCID 14798Sodium HydroxideHCID 15413tert-Butyl methyl etherHCID 178419564HCID 178419564, 화합물

생성물 1

HCID 230793905-Chloro-3-(ethylsulfanyl)-1,2,4-thiadiazole

실험 절차

To 60 ml of water, 10.3 g of ehtylisothiourea hydrobromide, 10.4 g of perchloromethylmercaptan were added, followed the solution of 9.39 g of sodium hydroxide dissolved to 60 ml of water was added dropwise slowly at about 0° C. Then, t-butylmethylether was added to the reaction mixture, and extracted. The organic layer was dried by anhydrous sodium salfate, and concentrated. The residue obtaind was subjected to silica gel column chromatography (hexanne:ethylacetate=30:1) to obtain 2.54 g of 3-ethylthio-5-chloro-1,2,4-thiadiazole.

후처리

  1. additionwas added dropwise slowly at about 0° C
  2. extractionextracted
  3. dry with materialThe organic layer was dried by anhydrous sodium salfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-93036e25438b436287b77393ef266a3f
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07342031B2

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