Water → 1-Crotyl-1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl) hydrazine

HRID 1589423ノート

反応式

HRID 1589423 の反応式
CN(C)C=O.[NH2:6][S:7]([C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][C:19]=1[Cl:20])[C:13]([NH:15][NH2:16])=[O:14])(=[O:9])=[O:8].[CH2:21](Br)[CH:22]=[CH:23][CH3:24].O>C(O)(C)C>[CH2:21]([N:16]([C:10]1[CH:11]=[CH:12][CH:17]=[CH:18][CH:19]=1)[NH:15][C:13](=[O:14])[C:12]1[CH:17]=[CH:18][C:19]([Cl:20])=[C:10]([S:7](=[O:9])(=[O:8])[NH2:6])[CH:11]=1)[CH:22]=[CH:23][CH3:24]

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 1224142-Butene, 1-bromo-HCID 24026562-Chloro-5-(hydrazinecarbonyl)benzene-1-sulfonamide

生成物 1

HCID 543987431-Crotyl-1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl) hydrazine

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

In a 250 ml round bottomed flask is placed 90 ml of N,N-dimethylformamide and 30 grams (0.092 mole) of 3-amino sulfonyl-4-chlorobenzhydrazide. The mixture was stirred to dissolve the solid, then 18.63 gms (0.138 mole) of crotyl bromide were added. The mixture was heated at 100° for 1.66 hours at which point TLC showed the reaction to be complete. The reaction mixture was cooled and diluted with 200 ml isopropanol. This solution was dripped into a slurry of 1.5 liters of ice and 4 liters of water. The solid which precipitated was collected, washed with water and air dried overnight, yielding the product which could be recrystallized from chloroform/carbon tetrachloride.

後処理

  1. customIn a 250 ml round bottomed flask is placed
  2. dissolutionto dissolve the solid
  3. temperatureThe mixture was heated at 100° for 1.66 hours at which point TLC
  4. customthe reaction
  5. temperatureThe reaction mixture was cooled
  6. customThe solid which precipitated
  7. customwas collected
  8. washwashed with water and air
  9. customdried overnight
  10. customyielding the product which
  11. customcould be recrystallized from chloroform/carbon tetrachloride

出典と根拠

ORDレコード
ord-c11cec87eff8428ba8b5fb41d79e3902
出典データセット
uspto-grants-1986_02
特許番号
US04570001

反応ノート

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