Butyl isocyanate → N-(n-butylcarbamoyl)-4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide

HRID 1638908

反応式

HRID 1638908 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)[C:10]=1[S:11]([NH2:14])(=[O:13])=[O:12])=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:27]([N:31]=[C:32]=[O:33])[CH2:28][CH2:29][CH3:30]>CC(C)=O>[CH2:27]([NH:31][C:32]([NH:14][S:11]([C:10]1[N:9]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)[N:8]=[CH:7][C:6]=1[C:4]([O:3][CH2:1][CH3:2])=[O:5])(=[O:13])=[O:12])=[O:33])[CH2:28][CH2:29][CH3:30]

参加物

5

反応物 3

HCID 8110Butyl isocyanateHCID 11430Potassium CarbonateHCID 140491554-Ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide

生成物 1

HCID 19839374N-(n-butylcarbamoyl)-4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide収率 95.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a 70 ml acetone mixture of 8.5 g of 4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide and 6.0 g of anhydrous potassium carbonate, added was 3.3 g of n-butylisocyanate at room temperature, followed by heating under reflux for 3 hours. After the reaction was completed, acetone was evaporated under reduced pressure, and then the residue was emptied into ice water to filter insolbles off, and then the filtrate was precipitated with hydrochloric acid. Crystals precipitated was filtered, washed with water and dried to obtain 10.8 g of N-(n-butylcarbamoyl)-4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide. m.p.: 180° to 181° C.

後処理

  1. additionadded
  2. customat room temperature
  3. temperatureby heating
  4. temperatureunder reflux for 3 hours
  5. customacetone was evaporated under reduced pressure
  6. filtrationto filter insolbles off, and then the filtrate
  7. customwas precipitated with hydrochloric acid
  8. customCrystals precipitated
  9. filtrationwas filtered
  10. washwashed with water
  11. customdried

出典と根拠

ORDレコード
ord-f49a1aa730cb47e18a9058c083cdc71e
出典データセット
uspto-grants-1989_11
特許番号
US04881965

関連ノート

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