Pyridine → 2,3,4-Trichloro-N-[3-(1H-tetrazol-5-yl)phenyl]benzenesulfonamide

HRID 589680ノート

反応式

HRID 589680 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[CH:5]=[CH:4][C:3]=1[S:10](Cl)(=[O:12])=[O:11].[NH2:14][C:15]1[CH:16]=[C:17]([C:21]2[NH:25][N:24]=[N:23][N:22]=2)[CH:18]=[CH:19][CH:20]=1.N1C=CC=CC=1>C(Cl)Cl>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[CH:5]=[CH:4][C:3]=1[S:10]([NH:14][C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([C:21]2[NH:25][N:24]=[N:23][N:22]=2)[CH:16]=1)(=[O:12])=[O:11]

参加物

5

反応物 3

HCID 1049PyridineHCID 369042,3,4-Trichlorobenzenesulfonyl chlorideHCID 178507542HCID 178507542、化合物

生成物 1

HCID 1785275052,3,4-Trichloro-N-[3-(1H-tetrazol-5-yl)phenyl]benzenesulfonamide収率 65%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 2,3,4-trichlorobenzenesulfonyl chloride (15 mg, 0.055 mmol), 5-(3-aminophenyl)tetrazole (8 mg, 0.05 mmol) and dry pyridine (12 μL) in CH2Cl2 (200 μL) was stirred at room temperature over night. The solvent was evaporated and the crude product was purified by preparative HPLC (ACE C8, 5 μm 21×50 mm, flow 25 ml/min, 50 mM NH4OAc in water/CH3CN) to give 13 mg (65%) of the title compound. MS (ESI+) calcd for C13H8Cl3N5O2S 402.946428, found 402.946188.

後処理

  1. customThe solvent was evaporated
  2. customthe crude product was purified by preparative HPLC (ACE C8, 5 μm 21×50 mm, flow 25 ml/min, 50 mM NH4OAc in water/CH3CN)

出典と根拠

ORDレコード
ord-6cf7232f46054717b933c3d50abe3712
出典データセット
uspto-grants-2016_01
特許番号
US09233946B2

反応ノート

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