Sulfuric Acid → 6-(2-Chloro-4-trifluoromethylphenoxy)-1,2,3-benzothiadiazole

HRID 64558노트

반응식

HRID 64558 반응식
C([S:8][C:9]1[CH:15]=[C:14]([O:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][C:18]=2[Cl:27])[CH:13]=[CH:12][C:10]=1[NH2:11])C1C=CC=CC=1.S(=O)(=O)(O)O.[N:33]([O-])=O.[Na+]>O>[Cl:27][C:18]1[CH:19]=[C:20]([C:23]([F:26])([F:25])[F:24])[CH:21]=[CH:22][C:17]=1[O:16][C:14]1[CH:13]=[CH:12][C:10]2[N:11]=[N:33][S:8][C:9]=2[CH:15]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 202362802-Benzylthio-4-(2-chloro-4-trifluoromethylphenoxy)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 202362796-(2-Chloro-4-trifluoromethylphenoxy)-1,2,3-benzothiadiazole

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3 g of 1C was added to an ice-cold solution of 50% aqueous sulfuric acid, and the mixture maintained below 10° C. during the addition of a solution of 0.7 g of sodium nitrite in 10 ml of water. This mixture was then stirred for 1 hour, allowed to reach ambient temperature, and then extracted with ether. The organic layer was separated, solvent removed and the resulting red oil chromatographically purified and recrystallized to yield 1, as a crystalline solid, m.p.: 72°-73° C.

후처리

  1. customto reach ambient temperature
  2. extractionextracted with ether
  3. customThe organic layer was separated
  4. customsolvent removed
  5. customthe resulting red oil chromatographically purified
  6. customrecrystallized
  7. customto yield 1

출처 및 근거

ORD 기록
ord-790d55d6419040eaac72634241915ea5
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609394

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