Water → 7-beta-Galactosylcoumarin-3-carboxylic acid

HRID 543866

反応式

HRID 543866 の反応式
[OH-].[K+].O.[C@@H:4]1([C:15]2[CH:24]=[C:23]3[C:18]([CH:19]=[C:20]([C:26]([O:28]CC)=[O:27])[C:21](=[O:25])[O:22]3)=[CH:17][CH:16]=2)[O:12][C@H:11]([CH2:13][OH:14])[C@H:9]([OH:10])[C@H:7]([OH:8])[C@H:5]1[OH:6]>CO>[C@@H:4]1([C:15]2[CH:24]=[C:23]3[C:18]([CH:19]=[C:20]([C:26]([OH:28])=[O:27])[C:21](=[O:25])[O:22]3)=[CH:17][CH:16]=2)[O:12][C@H:11]([CH2:13][OH:14])[C@H:9]([OH:10])[C@H:7]([OH:8])[C@H:5]1[OH:6]

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 22809745Ethyl 7-beta-galactosylcoumarin-3-carboxylate

生成物 1

HCID 228097447-beta-Galactosylcoumarin-3-carboxylic acid収率 97.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 24 g of potassium hydroxide, 80 ml of water, 240 ml of methanol, and 20 g (0.035 mol) of ethyl 7-β-galactosylcoumarin-3-carboxylate [Supra, Burd et al, Clin. Chem.] was prepared. The methanol was removed under reduced pressure. The concentrated aqueous solution was acidified to pH 2.6 with concentrated hydrochloric acid. The white precipitate was collected, washed with cold water, and recrystallized from hot water. The crystals were collected, washed with acetone, and dried at 80° C. for 1 hour. This gave 12 g (54% yield) of 7-β-galactosylcoumarin-3-carboxylic acid as white crystals, mp 250°-255° C.

後処理

  1. customwas prepared
  2. customThe methanol was removed under reduced pressure
  3. customThe white precipitate was collected
  4. washwashed with cold water
  5. customrecrystallized from hot water
  6. customThe crystals were collected
  7. washwashed with acetone
  8. customdried at 80° C. for 1 hour

出典と根拠

ORDレコード
ord-43b907e8715c46ecb4fb725e824a01a0
出典データセット
uspto-grants-1984_05
特許番号
US04447529

関連ノート

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