Sodium Hydroxide → 1,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

HRID 2304805ノート

反応式

HRID 2304805 の反応式
Br.Br[CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1.[OH-:22].[Na+]>O>[OH:22][CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 9866952HCID 9866952、化合物

生成物 1

HCID 99256571,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
20 °C

実験手順

50 g (0.118 mol of 3(R,S)-bromo-1-methyl-4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine hydrobromide (VI) were heated under reflux for 2 h in 100 ml of water. The reaction mixture was then cooled to 20° C. and adjusted to pH 12.5 by dropwise addition of 30 ml of 30% strength sodium hydroxide solution. After a short time, a pale brown precipitate crystallized out. The mixture was stirred at 5-10° C. for a further 1 h, and the precipitated product was filtered off with suction and washed with 30 ml of water. The crude product was then stirred with 20 ml of acetone, filtered off with suction and dried in vacuo.

後処理

  1. customAfter a short time, a pale brown precipitate crystallized out
  2. filtrationthe precipitated product was filtered off with suction
  3. washwashed with 30 ml of water
  4. stirringThe crude product was then stirred with 20 ml of acetone
  5. filtrationfiltered off with suction
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-1a8b261ef9224735a513c0e567f765c9
出典データセット
uspto-grants-2002_08
特許番号
US06437136B1

反応ノート

読み込み中…