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

HRID 374752
ノート
印刷プレビュー

反応式

HRID 374752 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 178519022HCID 178519022、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-56dd81d6255f4c6587839133ba77d804
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05482916

反応ノート

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