Lithium Hydroxide → 4-(Biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acid

HRID 460042ノート

反応式

HRID 460042 の反応式
[OH-].[Li+].C[O:4][C:5]([C:7]1[O:8][C:9]([CH3:26])=[C:10]([CH2:12][O:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:16][CH:15]=2)[CH:11]=1)=[O:6]>O1CCCC1.CO>[C:17]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:16]=[CH:15][C:14]([O:13][CH2:12][C:10]2[CH:11]=[C:7]([C:5]([OH:6])=[O:4])[O:8][C:9]=2[CH3:26])=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 588241734-(Biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acid methyl ester

生成物 1

HCID 7868594-(Biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acid収率 22%

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

1M Aqueous lithium hydroxide (18 mL) was added to solution of 4-(biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acid methyl ester (17) (1 g) in tetrahydrofuran/methanol (2:1 by volume, 100 mL) and the mixture stirred at room temperature for 5 h. The solvent was removed in vacuo, the residue dissolved in water (20 mL) and the solution acidified to pH6 with aqueous dilute hydrochloric acid. The mixture was evaporated to dryness and the residue was purified by HPLC to afford compound 18 as a white solid (210 mg). LC/MS System B: Rt=4.80 mins, m/z=307 ((M−1) for C19H16O4).

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in water (20 mL)
  3. customThe mixture was evaporated to dryness
  4. customthe residue was purified by HPLC

出典と根拠

ORDレコード
ord-adede7104c1646fc96ab731ee9893133
出典データセット
uspto-grants-2007_03
特許番号
US07196089B2

反応ノート

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