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Hydrochloric Acid → 5-Isopropyl-pyridine-2-sulfonic acid [4-(3-nitro-phenyl)-thiazol-2-yl]-amide

HRID 619035
ノート
印刷プレビュー

反応式

HRID 619035 の反応式
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].[CH:17]([C:20]1[CH:21]=[CH:22][C:23]([S:26](Cl)(=[O:28])=[O:27])=[N:24][CH:25]=1)([CH3:19])[CH3:18].Cl>N1C=CC=CC=1>[N+:2]([C:5]1[CH:6]=[C:7]([C:11]2[N:12]=[C:13]([NH:16][S:26]([C:23]3[CH:22]=[CH:21][C:20]([CH:17]([CH3:19])[CH3:18])=[CH:25][N:24]=3)(=[O:27])=[O:28])[S:14][CH:15]=2)[CH:8]=[CH:9][CH:10]=1)([O-:4])=[O:3]
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 218455864-(3-Nitrophenyl)thiazol-2-amine hydrochlorideHCID 222819185-Isopropylpyridine-2-sulfonyl chloride

生成物 1

HCID 867537545-Isopropyl-pyridine-2-sulfonic acid [4-(3-nitro-phenyl)-thiazol-2-yl]-amide収率 39.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 0.5 g of 4-(3-nitro-phenyl)-thiazol-2-ylamine hydrochloride with 0.46 g of 5-isopropyl-pyridine-2-sulfonyl 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 40 ml of ethanol and 20 ml of ethyl acetate yielded 0.31 g of 5-isopropyl-pyridine-2-sulfonic acid [4-(3-nitro-phenyl)-thiazol-2-yl]-amide as yellowish crystals.

後処理

  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 40 ml of ethanol and 20 ml of ethyl acetate

出典と根拠

ORDレコード
ord-1e202543db3340a58d9c937d4c27f199
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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