P-Toluenesulfonylhydrazide → 4-Cyano-2-(2-(3,4-dichlorophenyl)ethylsulfonamido)benzenesulfonamide

HRID 2283317노트

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HRID 2283317 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:5]([NH:13][S:14](/[CH:17]=[CH:18]/[C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=2)(=[O:16])=[O:15])[CH:4]=1)#[N:2].C([O-])(=O)C.[Na+].C1(C)C=CC(S(NN)(=O)=O)=CC=1>O1CCCC1>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([S:9]([NH2:12])(=[O:10])=[O:11])=[C:5]([NH:13][S:14]([CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=2)(=[O:16])=[O:15])[CH:4]=1)#[N:2]

참가 물질

5

반응물 3

HCID 15303P-ToluenesulfonylhydrazideHCID 517045Sodium AcetateHCID 57750965(E)-4-Cyano-2-(2-(3,4-dichlorophenyl)vinylsulfonamido)benzenesulfonamide

생성물 1

HCID 577510914-Cyano-2-(2-(3,4-dichlorophenyl)ethylsulfonamido)benzenesulfonamide수율 4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
180 °C

실험 절차

(E)-4-Cyano-2-(2-(3,4-dichlorophenyl)vinylsulfonamido)benzenesulfonamide (123 mg, 0.28 mmol), sodium acetate (93 mg, 1.14 mmol) and para-toluenesulfonhydrazide (212 mg, 1.14 mmol) were dissolved in anhydrous tetrahydrofuran (3 mL) in a microwave vial. The vial was capped and evacuated two times with argon. The mixture was heated in a microwave at 180° C. for 15 min. The mixture was filtered and the solvent was evaporated in vacuo. Purification twice by preparative HPLC gave 4.8 mg (4% yield) of the title compound.

후처리

  1. customThe vial was capped
  2. customevacuated two times with argon
  3. filtrationThe mixture was filtered
  4. customthe solvent was evaporated in vacuo
  5. customPurification twice by preparative HPLC

출처 및 근거

ORD 기록
ord-224f0dfa8fda4579bc3ee406a3a89493
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145380B2

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