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Water → 4-(2,6-Dichlorophenyl)-1,2,5-thiadiazol-3-yl acetate

HRID 1078182
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반응식

HRID 1078182 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:13]([OH:14])=[N:12][S:11][N:10]=1.N1C=CC=CC=1.[C:21](OC(=O)C)(=[O:23])[CH3:22].O>CCOCC>[C:21]([O:14][C:13]1[C:9]([C:3]2[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=2[Cl:8])=[N:10][S:11][N:12]=1)(=[O:23])[CH3:22]
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참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 178519022HCID 178519022, 화합물

생성물 1

HCID 194291224-(2,6-Dichlorophenyl)-1,2,5-thiadiazol-3-yl acetate수율 70.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

In ether, 0.5 g of 3-(2,6-dichlorophenyl)-4-hydroxy-1,2,5-thiadiazole and 0.18 g of pyridine were dissolved and 0.23 g of acetic anhydride was added thereto. The mixture was stirred for 3 hours at room temperature. The reaction mixture was poured into water and extracted with ether. The ether layer was washed twice with aqueous dilute sodium hydroxide solution, twice with water and twice with aqueous saturated sodium chloride solution. The resultant was dried over anhydrous sodium sulfate and concentrated, followed by silica gel column chromatography to obtain 0.41 g of 4-(2,6-dichlorophenyl)-1,2,5-thiadiazol-3-yl acetate.

후처리

  1. extractionextracted with ether
  2. washThe ether layer was washed twice with aqueous dilute sodium hydroxide solution, twice with water and twice with aqueous saturated sodium chloride solution
  3. dry with materialThe resultant was dried over anhydrous sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b36ecd01d7df4e2a8e08b63285489174
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05547920

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