tert-Butyl-3-aminobenzoate → 3-(Pyridine-3-sulfonylamino)-benzoic acid tert-butyl ester

HRID 62816

反応式

HRID 62816 の反応式
[C:1]([O:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH2:13])[CH:8]=1)([CH3:4])([CH3:3])[CH3:2].[N:15]1[CH:20]=[CH:19][CH:18]=[C:17]([S:21](Cl)(=[O:23])=[O:22])[CH:16]=1>N1C=CC=CC=1.C1(C)C=CC=CC=1>[C:1]([O:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][S:21]([C:17]2[CH:16]=[N:15][CH:20]=[CH:19][CH:18]=2)(=[O:23])=[O:22])[CH:8]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 2737408tert-Butyl-3-aminobenzoateHCID 3164136Pyridine-3-sulfonyl chloride

生成物 1

HCID 673108723-(Pyridine-3-sulfonylamino)-benzoic acid tert-butyl ester収率 104.7%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 1140Toluene溶媒

実験手順

A solution of tert-butyl-3-aminobenzoate (100 mg, 0.5 mmol) and pyridine-3-sulfonylchloride (110 mg, 0.5 mmol) in pyridine (5 ml) was heated to 50° C. for 90 min. On cooling, the reaction was diluted with toluene (100 ml) and concentrated in vacuo. This was repeated with further aliquots of toluene until all the pyridine had been removed to afford the title compound as a yellow oil (175 mg). HPLC retention time 4.27 min. Mass spectrum (ES+) m/z 335 (M+H).

後処理

  1. temperatureOn cooling
  2. concentrationconcentrated in vacuo
  3. customhad been removed

出典と根拠

ORDレコード
ord-7d115dd033a8422f9a090d4e1b705403
出典データセット
uspto-grants-2016_09
特許番号
US09447033B2

関連ノート

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