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

HRID 2225833ノート

反応式

HRID 2225833 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a54f42d2d8fd4dbaa6deb86e846a3d40
出典データセット
uspto-grants-1994_09
特許番号
US05344843

反応ノート

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