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

HRID 2283317ノート

反応式

HRID 2283317 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
180 °C

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-224f0dfa8fda4579bc3ee406a3a89493
出典データセット
uspto-grants-2015_09
特許番号
US09145380B2

反応ノート

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