4-Toluenesulfonyl chloride → 4-Propionylpyridine oxime tosylate

HRID 371400ノート

反応式

HRID 371400 の反応式
[C:1](=[N:10][OH:11])([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)[CH2:2][CH3:3].[C:12]1([CH3:22])[CH:17]=[CH:16][C:15]([S:18](Cl)(=[O:20])=[O:19])=[CH:14][CH:13]=1>N1C=CC=CC=1>[S:18]([C:15]1[CH:16]=[CH:17][C:12]([CH3:22])=[CH:13][CH:14]=1)([OH:11])(=[O:20])=[O:19].[C:1](=[N:10][OH:11])([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)[CH2:2][CH3:3]

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 1363417421-(Pyridin-4-yl)propan-1-one oxime

生成物 1

HCID 1363872634-Propionylpyridine oxime tosylate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To the oxime 2 of Example 2 (5.0 g, 33 mmol) dissolved in pyridine (31 mL) was added p-toluenesulfonyl chloride (7.4 g, 39 mmol) and the reaction mixture stirred at room temperature for 24 hours. Pyridine hydrochloride was removed by filtration and the filtrate concentrated under reduced pressure. The solid obtained was slurried in hexanes, filtered, and air dried to give the compound 3 as a pale peach-colored solid: NMR (CDCl3) δ 1.12 (t, 3H, J=8 Hz), 2.45 (s, 3H), 2.81 (q, 2H, J=8 Hz), and 7.27-7.98 (m, 8H).

後処理

  1. customPyridine hydrochloride was removed by filtration
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe solid obtained
  4. filtrationfiltered
  5. customair dried

出典と根拠

ORDレコード
ord-f2d87eba931649f592dc6d67dec8dc33
出典データセット
uspto-grants-1985_07
特許番号
US04532250

反応ノート

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