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

HRID 1589423노트

반응식

HRID 1589423 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c11cec87eff8428ba8b5fb41d79e3902
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04570001

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