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

HRID 1819974노트

반응식

HRID 1819974 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-33b979f09ee443f1b1deb1414f8522a7
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601873B2

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