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

HRID 64558ノート

反応式

HRID 64558 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-790d55d6419040eaac72634241915ea5
出典データセット
uspto-grants-1986_09
特許番号
US04609394

反応ノート

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