Hydrochloric Acid → 3,4-Dichloro-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide

HRID 619033

반응식

HRID 619033 반응식
Cl.[N+:2]([C:5]1[CH:6]=[C:7]([C:11]2[N:12]=[C:13]([NH2:16])[S:14][CH:15]=2)[CH:8]=[CH:9][CH:10]=1)([O-:4])=[O:3].[Cl:17][C:18]1[CH:19]=[C:20]([S:25](Cl)(=[O:27])=[O:26])[CH:21]=[CH:22][C:23]=1[Cl:24].Cl>N1C=CC=CC=1>[Cl:17][C:18]1[CH:19]=[C:20]([S:25]([NH:16][C:13]2[S:14][CH:15]=[C:11]([C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([N+:2]([O-:4])=[O:3])[CH:6]=3)[N:12]=2)(=[O:26])=[O:27])[CH:21]=[CH:22][C:23]=1[Cl:24]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 218455864-(3-Nitrophenyl)thiazol-2-amine hydrochloride

생성물 1

HCID 105266133,4-Dichloro-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide수율 46.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 0.5 g of 4-(3-nitro-phenyl)-thiazol-2-ylamine hydrochloride with 0.52 g of 3,4-dichlorobenzenesulfonyl chloride was stirred overnight with 2 ml of pyridine. The resulting, red colored suspension was poured into 25 ml of 1N hydrochloric acid and the solid which thereby separated was filtered off and dissolved in a mixture of 30 ml of ethanol and 20 ml of 2N sodium hydroxide solution. After the addition of 0.5 g of active charcoal the mixture was stirred at room temperature for 30 minutes and subsequently the active charcoal was filtered off. The product separated upon neutralization with concentrated hydrochloric acid. Recrystallization from 80 ml of 50% ethanol yielded 0.39 g of 3,4-dichloro-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide as yellowish crystals.

후처리

  1. customthe solid which thereby separated
  2. filtrationwas filtered off
  3. dissolutiondissolved in a mixture of 30 ml of ethanol and 20 ml of 2N sodium hydroxide solution
  4. additionAfter the addition of 0.5 g of active charcoal the mixture
  5. filtrationsubsequently the active charcoal was filtered off
  6. customThe product separated upon neutralization with concentrated hydrochloric acid
  7. customRecrystallization from 80 ml of 50% ethanol

출처 및 근거

ORD 기록
ord-9eb2dc07101942c9a7c87711103fa45f
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958910

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