Sulfuric Acid → 5-Chloro-2,1,3-benzothiadiazole

HRID 1819974ノート

反応式

HRID 1819974 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([NH2:9])[CH:3]=1.[S:10](Cl)(Cl)=O.S(=O)(=O)(O)O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2=[N:8][S:10][N:9]=[C:4]2[CH:3]=1

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 72634-Chloro-1,2-diaminobenzeneHCID 24386Thionyl Chloride

生成物 1

HCID 2841235-Chloro-2,1,3-benzothiadiazole

実験手順

A mixture was prepared by mixing 4.0 g (28 mmol) of 4-chloro-o-phenylenediamine, 14 mL of thionyl chloride and 0.62 mL of concentrated sulfuric acid and was refluxed for one hour. This mixture was cooled and then poured onto ice, and a resultant precipitate was filtered and collected. This precipitate was washed with water till the waste water became neutral and then thoroughly dried to yield 4.6 g of 5-chloro-2,1,3-benzothiadiazole as a crude product (melting point, 50 to 54° C.; yield, 96%). This crude product was vacuum-distilled to yield a pure product of 5-chloro-2,1,3-benzothiadiazole (melting point, 54° C.; yield, 85%).

後処理

  1. customA mixture was prepared
  2. temperaturewas refluxed for one hour
  3. temperatureThis mixture was cooled
  4. additionpoured onto ice
  5. filtrationa resultant precipitate was filtered
  6. customcollected
  7. washThis precipitate was washed with water till the waste water
  8. customthoroughly dried

出典と根拠

ORDレコード
ord-33b979f09ee443f1b1deb1414f8522a7
出典データセット
uspto-grants-2009_10
特許番号
US07601873B2

反応ノート

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