Sodium Hydroxide → Pranoprofen

HRID 1579451

반응식

HRID 1579451 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 4888Pranoprofen수율 58.7%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 178418361HCID 178418361, 화합물용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e74532c36a8742fbac5be2082ad23742
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931205

연결된 노트

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