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Hydrochloric Acid → HCID 21845571、化合物

HRID 619068
ノート
印刷プレビュー

反応式

HRID 619068 の反応式
Br.[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].[Br:17][C:18]1[CH:19]=[C:20]([S:26](Cl)(=[O:28])=[O:27])[CH:21]=[CH:22][C:23]=1[O:24][CH3:25].Cl>N1C=CC=CC=1>[Br:17][C:18]1[CH:19]=[C:20]([S:26]([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:28])=[O:27])[CH:21]=[CH:22][C:23]=1[O:24][CH3:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 28704454-(3-Nitro-phenyl)-thiazol-2-ylamine hydrobromideHCID 38637473-bromo-4-methoxybenzenesulfonyl chloride

生成物 1

HCID 21845571HCID 21845571、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 5.0 g of 4-(3-nitro-phenyl)-thiazol-2-ylamine hydrobromide with 5.2 g of 3-bromo-4-methoxy-benzene-sulfonyl chloride was stirred for 3 hours with 20 ml of pyridine. The resulting, red colored suspension was poured into 300 ml of 1N hydrochloric acid and the mixture was extracted with ethyl acetate. The organic phase was dried with magnesium sulphate and concentrated. The residue was dissolved in a mixture of 300 ml of ethanol and 200 ml of 2N sodium hydroxide solution. After the addition of 4.5 g of active charcoal the mixture was stirred at room temperature for 30 minutes and subsequently the active charcoal was filtered off. 4.4 g of 3-bromo-4-methoxy-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide separated as yellow crystals upon neutralization with concentrated hydrochloric acid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic phase was dried with magnesium sulphate
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in a mixture of 300 ml of ethanol and 200 ml of 2N sodium hydroxide solution
  5. additionAfter the addition of 4.5 g of active charcoal the mixture
  6. filtrationsubsequently the active charcoal was filtered off
  7. custom4.4 g of 3-bromo-4-methoxy-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide separated as yellow crystals upon neutralization with concentrated hydrochloric acid

出典と根拠

ORDレコード
ord-3c3fa808bf494dd694660a02abd92103
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05958910

反応ノート

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