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

HRID 543866

반응식

HRID 543866 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 228097447-beta-Galactosylcoumarin-3-carboxylic acid수율 97.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-43b907e8715c46ecb4fb725e824a01a0
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04447529

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