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

HRID 1417270노트

반응식

HRID 1417270 반응식
Br.[N+:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[N:12]=[C:13]([NH2:16])[S:14][CH:15]=1)([O-:4])=[O:3].[C:17]1([CH3:27])[CH:22]=[CH:21][C:20]([S:23](Cl)(=[O:25])=[O:24])=[CH:19][CH:18]=1.Cl>N1C=CC=CC=1>[CH3:27][C:17]1[CH:22]=[CH:21][C:20]([S:23]([NH:16][C:13]2[S:14][CH:15]=[C:11]([C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=3[N+:2]([O-:4])=[O:3])[N:12]=2)(=[O:25])=[O:24])=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 218455924-(2-Nitro-phenyl)-thiazol-2-ylamine hydrobromide

생성물 1

HCID 218455994-Methyl-N-[4-(2-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 0.5 g of 4-(2-nitro-phenyl)-thiazol-2-ylamine hydrobromide with 0.47 g of p-toluenesulfonyl chloride was stirred overnight with 2 ml of pyridine. The resulting, red colored suspension was poured into 30 ml of 1N hydrochloric acid and extracted twice with 40 ml of ethyl acetate each time. The organic extracts were combined, dried with magnesium sulphate and concentrated. The residue was dissolved in a mixture of 30 ml of ethanol and 20 ml of 2N sodium hydroxide solution. After the addition of 0.4 g of active charcoal the mixture was stirred at room temperature for 30 minutes and subsequently the active charcoal was filtered off. After neutralization with concentrated hydrochloric acid and boiling there separated, upon cooling, 0.58 g of 4-methyl-N-[4-(2-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide as yellow crystals.

후처리

  1. extractionextracted twice with 40 ml of ethyl acetate each time
  2. dry with materialdried with magnesium sulphate
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in a mixture of 30 ml of ethanol and 20 ml of 2N sodium hydroxide solution
  5. additionAfter the addition of 0.4 g of active charcoal the mixture
  6. filtrationsubsequently the active charcoal was filtered off
  7. customAfter neutralization with concentrated hydrochloric acid and boiling there separated
  8. temperatureupon cooling

출처 및 근거

ORD 기록
ord-e3563b45dbd14165bc552a49d9cabeae
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05877193

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