Sodium Hydroxide → 4-[3-[4-Carboxy-3-hydroxy-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid

HRID 2225833노트

반응식

HRID 2225833 반응식
[OH:1][C:2]1[C:3]([CH2:28][CH2:29][CH3:30])=[C:4]([CH:21]=[CH:22][C:23]=1[C:24]([O:26]C)=[O:25])[O:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](=[O:20])[C:17]([OH:19])=[O:18])=[CH:12][CH:11]=1.[OH-].[Na+]>CO>[C:24]([C:23]1[CH:22]=[CH:21][C:4]([O:5][CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16](=[O:20])[C:17]([OH:19])=[O:18])=[CH:12][CH:11]=2)=[C:3]([CH2:28][CH2:29][CH3:30])[C:2]=1[OH:1])([OH:26])=[O:25]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 190044424-[3-[3-Hydroxy-4-(methoxycarbonyl)-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid

생성물 1

HCID 190044864-[3-[4-Carboxy-3-hydroxy-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4-[3-[3-hydroxy-4-(methoxycarbonyl)-2-propylphenoxy)propoxy]-alphaoxobenzeneacetic acid (0.3 g) in methanol (30 mL) was treated with 4N sodium hydroxide (0.58 mL) was stirred at reflux for 46 hours. The methanol was removed in vacuo, then the mixture was acidified with 3N hydrochloric acid and extracted with dichloromethane-tetrahydrofuran (1:1). The dried (MgSO4) extracts were evaporated and the solid residue was crystallized from dichloromethane-hexane, and then from acetone-hexane to afford 4-[3-[4-carboxy-3-hydroxy-2-propylphenoxy)propoxy]-alpha-oxobenzeneacetic acid, mp 182°-185° C.

후처리

  1. temperatureat reflux for 46 hours
  2. customThe methanol was removed in vacuo
  3. extractionextracted with dichloromethane-tetrahydrofuran (1:1)
  4. dry with materialThe dried (MgSO4) extracts
  5. customwere evaporated
  6. customthe solid residue was crystallized from dichloromethane-hexane

출처 및 근거

ORD 기록
ord-a54f42d2d8fd4dbaa6deb86e846a3d40
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

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