Hydrochloric Acid → N-(Butylcarbamoyl)-4-nitrothiophene-2-sulfonamide

HRID 434598ノート

反応式

HRID 434598 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([S:9]([NH2:12])(=[O:11])=[O:10])[S:7][CH:8]=1)([O-:3])=[O:2].[CH2:13]([N:17]=[C:18]=[O:19])[CH2:14][CH2:15][CH3:16].C(=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O>[CH2:13]([NH:17][C:18]([NH:12][S:9]([C:6]1[S:7][CH:8]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)(=[O:10])=[O:11])=[O:19])[CH2:14][CH2:15][CH3:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8110Butyl isocyanateHCID 11430Potassium CarbonateHCID 202157164-Nitro-2-thiophenesulfonamide

生成物 1

HCID 20215715N-(Butylcarbamoyl)-4-nitrothiophene-2-sulfonamide

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A stirred suspension of 10 g of 4-nitrothiophene-2-sulfonamide, 6 g of n-butyl isocyanate and 7 g of anhydrous potassium carbonate in 100 ml of acetone was heated to reflux for 3 hours. The resultant viscous mixture was poured into ice-water and the pH adjusted to 2 by the addition of concentrated hydrochloric acid. The resulting tarry precipitate thus obtained was extracted into methylene chloride, separated from the aqueous phase, dried over magnesium sulfate, filtered and concentrated in-vacuo. The residue which showed absorption peaks by NMR at 0.7 to 1.7 (multiplet), consistent for butyl and at 8.3 and 8.5, consistent for the thiophene ring was used without further purification in the following example.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 3 hours
  3. customThe resulting tarry precipitate thus obtained
  4. extractionwas extracted into methylene chloride
  5. customseparated from the aqueous phase
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in-vacuo
  9. customabsorption peaks by NMR at 0.7 to 1.7 (multiplet)

出典と根拠

ORDレコード
ord-c0eca668e4754635bf9a2942cceee468
出典データセット
uspto-grants-1983_08
特許番号
US04398939

反応ノート

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