Tert-Butylamine → 2-(4-Nitro-phenyl)-ethanesulfonic acid tert-butylamide

HRID 1711288ノート

反応式

HRID 1711288 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[N+:6]([C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][S:17](Cl)(=[O:19])=[O:18])=[CH:11][CH:10]=1)([O-:8])=[O:7]>C1COCC1>[C:1]([NH:5][S:17]([CH2:16][CH2:15][C:12]1[CH:13]=[CH:14][C:9]([N+:6]([O-:8])=[O:7])=[CH:10][CH:11]=1)(=[O:18])=[O:19])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 27611752-(4-nitrophenyl)ethanesulfonyl Chloride

生成物 1

HCID 685055592-(4-Nitro-phenyl)-ethanesulfonic acid tert-butylamide収率 62%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of tert-BuNH2 (15.6 mL, 148 mmol) in THF (50 mL) at 0° C., 2-(4-nitro-phenyl)-ethanesulfonyl chloride (WO 2006010079, 1.9 g, 7.6 mmol) was added portionwise. The resulting mixture was stirred for 24 h at RT. The solvent was removed in vacuo and the residue was taken up in DCM (50 mL) and cold 0.5 N HCl (50 mL). The organic layer was separated, dried (Na2SO4) and concentrated to obtain 2-(4-nitro-phenyl)-ethanesulfonic acid tert-butylamide (1.3 g, 62%) which was used directly without further purification.

後処理

  1. customThe solvent was removed in vacuo
  2. customThe organic layer was separated
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-104fb777ceed4c918a161632e419da38
出典データセット
uspto-grants-2010_09
特許番号
US07790724B2

反応ノート

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