Hydrochloric Acid → 1,6-Dimethyl-2-(1-methoxypropyl)-3-hydroxy-pyridin-4(1H)-one hydrochloride

HRID 1249804ノート

反応式

HRID 1249804 の反応式
[CH3:1][N:2]1[C:7]([CH3:8])=[CH:6][C:5](=[O:9])[C:4]([O:10]CC2C=CC=CC=2)=[C:3]1[CH:18]([O:21][CH3:22])[CH2:19][CH3:20].[ClH:23]>CO.O.[Pd]>[ClH:23].[CH3:1][N:2]1[C:7]([CH3:8])=[CH:6][C:5](=[O:9])[C:4]([OH:10])=[C:3]1[CH:18]([O:21][CH3:22])[CH2:19][CH3:20]

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 186787911,6-Dimethyl-2-(1-methoxypropyl)-3-benzyloxy-pyridin-4(1H)-one

生成物 1

HCID 186788091,6-Dimethyl-2-(1-methoxypropyl)-3-hydroxy-pyridin-4(1H)-one hydrochloride収率 79.3%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

1,6-Dimethyl-2-(1-methoxypropyl)-3-benzyloxy-pyridin-4-(1H)-one (1.65 g, 5.5 mmol) was dissolved in methanol (30 ml)/water (10 ml) and adjusted to pH 1 with concentrated hydrochloric acid prior to hydrogenolysis for 4 hours in the presence of 5% Pd/C catalyst (0.35 g). Filtration followed by rotary evaporation gave the crude product as a white solid. Recrystallization from methanol/diethyl ether gave the pure title compound (1.08 g, 79.3%) as a white crystalline solid. m.p. 225-227° C.

後処理

  1. filtrationFiltration
  2. customfollowed by rotary evaporation
  3. customgave the crude product as a white solid
  4. customRecrystallization from methanol/diethyl ether

出典と根拠

ORDレコード
ord-1132c3a5cf634e7097eb14ad8617d0ad
出典データセット
uspto-grants-2002_01
特許番号
US06335353B1

反応ノート

読み込み中…