Hydroxyamine hydrochloride → 5-p-Methoxybenzyloxy-1-hydroxy-2-hydroxymethyl-4-pyridone

HRID 627291ノート

反応式

HRID 627291 の反応式
[OH:1][CH2:2][C:3]1O[CH:5]=[C:6]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[C:7](=[O:9])[CH:8]=1.Cl.[NH2:21][OH:22]>N1C=CC=CC=1>[OH:22][N:21]1[CH:5]=[C:6]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[C:7](=[O:9])[CH:8]=[C:3]1[CH2:2][OH:1]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 104916984H-Pyran-4-one, 2-(hydroxymethyl)-5-[(4-methoxyphenyl)methoxy]-2 回

生成物 1

HCID 107076455-p-Methoxybenzyloxy-1-hydroxy-2-hydroxymethyl-4-pyridone収率 38.3%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
85 °C

実験手順

To a stirred solution of 2-(hydroxymethyl)-5-[(4-methoxybenzyl)oxy]-4H-pyran-4-one (Intermediate 289, 101.7 g, 0.388 mol) in pyridine (1.35 L) was added hydroxylamine hydrochloride (134.7 g, 1.94 mol). The reaction mixture was heated at 85° C. for 4 hours, then evaporated to dryness and triturated with water (700 mL). The precipitate was collected by filtration and washed with water (250 mL). The solids were then stirred in isopropanol (100 mL) for 12 hours, collected by filtration and dried under vacuum to afford the title compound as a white solid (41.2 g, 38%).

後処理

  1. customevaporated to dryness
  2. customtriturated with water (700 mL)
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water (250 mL)
  5. filtrationcollected by filtration
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-fdbc379c943a4301bea49dcc4d69b882
出典データセット
uspto-grants-2016_04
特許番号
US09309245B2

反応ノート

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