Water → 5-Bromo-N-(tert-butyl)pyridine-2-sulfonamide

HRID 1772661ノート

反応式

HRID 1772661 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8](Cl)(=[O:10])=[O:9])=[N:6][CH:7]=1.[C:12]([NH2:16])([CH3:15])([CH3:14])[CH3:13].O>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([NH:16][C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:10])=[O:9])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 6385Tert-ButylamineHCID 445580975-Bromopyridine-2-sulfonyl chloride

生成物 1

HCID 711166495-Bromo-N-(tert-butyl)pyridine-2-sulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 5-bromopyridine-2-sulfonyl chloride (2.7 g, 10 mmol) in DCM (100 mL) was cooled to 0° C. and treated with tert-BuNH2 (5.5 mL, 52 mmol). The resulting mixture was stirred at rt for 48 h. Water (50 mL) was added and the DCM layer were separated, dried and concentrated to obtain compound 32a. 1H-NMR (400 MHz, CDCl3) δ (ppm): 8.75 (d, J=2.3 Hz, 1H), 8.03 (dd, J=8.2, 2.3 Hz, 1H), 7.90-7.94 (m, 1H), 5.02-5.07 (m, 1H), 1.23 (s, 9H).

後処理

  1. customthe DCM layer were separated
  2. customdried
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-ecd019b54a7644189cf319967949951e
出典データセット
uspto-grants-2016_02
特許番号
US09249163B2

反応ノート

読み込み中…