(6-Chloro-4-(methylamino)pyridin-3-yl)methanol → 6-Chloro-4-(methylamino)nicotinaldehyde

HRID 524051ノート

反応式

HRID 524051 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([NH:10][CH3:11])[CH:3]=1>ClCCl.C1COCC1.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[CH:3]=[C:4]([NH:10][CH3:11])[C:5]([CH:8]=[O:9])=[CH:6][N:7]=1

参加物

5

反応物 1

HCID 51000240(6-Chloro-4-(methylamino)pyridin-3-yl)methanol

生成物 1

HCID 234345716-Chloro-4-(methylamino)nicotinaldehyde収率 87.8%

試薬・触媒・溶媒 3

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of (6-chloro-4-(methylamino)pyridin-3-yl)methanol (4.2 g, 24.7 mmol) and manganese(IV) oxide (active, 25.8 g, 296.6 mmol) in dichloromethane (50 mL) and THF (50 mL) was stirred at RT overnight. LCMS showed the reaction was completed. The solid was filtered off, and the filtrate was concentrated to afford the title compound (3.7 g, crude) as a light yellow solid, which was directly used in the next step without further purification. MS (ES+) C7H7ClN2O requires: 170, 172. found: 171, 173 [M+H]+.

後処理

  1. filtrationThe solid was filtered off
  2. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-91f62f4b2cc8480080b516bf35366868
出典データセット
uspto-grants-2016_05
特許番号
US09340514B2

反応ノート

読み込み中…