Sodium Hydroxide → Pranoprofen

HRID 1579451

反応式

HRID 1579451 の反応式
Cl[C:2]([C:7]1[CH:8]=[CH:9][C:10]2[O:19][C:14]3=[N:15][CH:16]=[CH:17][CH:18]=[C:13]3[CH2:12][C:11]=2[CH:20]=1)([CH3:6])[C:3]([OH:5])=[O:4].[OH-].[Na+]>[Ni].[H][H]>[N:15]1[CH:16]=[CH:17][CH:18]=[C:13]2[CH2:12][C:11]3[CH:20]=[C:7]([CH:2]([CH3:6])[C:3]([OH:5])=[O:4])[CH:8]=[CH:9][C:10]=3[O:19][C:14]=12

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 215685142-chloro-2-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)propionic acid

生成物 1

HCID 4888Pranoprofen収率 58.7%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 178418361HCID 178418361、化合物溶媒2 回

実験手順

A mixture of 2.9 g of 2-chloro-2-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)propionic acid, 40 ml of 0.5 N aqueous sodium hydroxide solution and 1 g of Raney nickel is stirred in a hydrogen stream at ordinary pressure and temperature, until absorption of 230 ml of hydrogen is attained. The RAney nickel is then filtered off, and the filtrate is neutralized with hydrochloric acid. The crystalline precipitate is filtered off, washed with water, and recrystallized from aqueous dioxane to give 1.5 g of 2-(5H-[1]benzopyrano-[2,3-b]pyridin-7-yl)propionic acid melting at 183°-184°C.

後処理

  1. filtrationThe RAney nickel is then filtered off
  2. filtrationThe crystalline precipitate is filtered off
  3. washwashed with water
  4. customrecrystallized from aqueous dioxane

出典と根拠

ORDレコード
ord-e74532c36a8742fbac5be2082ad23742
出典データセット
uspto-grants-1976_01
特許番号
US03931205

関連ノート

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