Hydrochloric Acid → 2-(4-Chlorobenzoylamino)-3-(oxindol-3-yl)propionic acid monohydrate

HRID 2309251

Reaktionsgleichung

Reaktionsgleichung von HRID 2309251
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([NH:8][CH:9]([CH2:13][C:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][CH:15]=2)[C:10]([OH:12])=[O:11])=[O:7])=[CH:4][CH:3]=1.Cl.[OH2:26].CO>CS(C)=O.C(Cl)(Cl)Cl>[OH2:7].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([NH:8][CH:9]([CH2:13][CH:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][C:15]2=[O:26])[C:10]([OH:12])=[O:11])=[O:7])=[CH:23][CH:24]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric Acid2×HCID 887MethanolHCID 962WaterHCID 27875262-[(4-chlorophenyl)formamido]-3-(1H-indol-3-yl)propanoic acid

Produkt 1

HCID 133932552-(4-Chlorobenzoylamino)-3-(oxindol-3-yl)propionic acid monohydrate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

6.8 Grams of 2-(4-chlorobenzoylamino)-3-(indol-3-yl)propionic acid prepared in Reference Example 6 was suspended in 8 g of dimethyl sulfoxide, then 17 g of concentrated hydrochloric acid was added to the suspension, and the resulting mixture was stirred at a room temperature for 2 hours. Further, 80 ml of water was added to the reaction mixture and stirred at a room temperature for 1 hour. The crystals formed were collected by filtration, washed with water, and dried. The crude crystals thus obtained were suspended in a mixture of chloroform:methanol=50:1 and stirred, the crystals were collected by filtration, and dissolved in a saturated sodium bicarbonate aqueous solution. The insoluble materials were removed by filtration, the filtrate obtained was neutralized with 10%-hydrochloric acid. The crystals formed were collected by filtration, washed with water, dried to obtain 3.2 g of 2-(4-chlorobenzoylamino)-3-(oxindol-3-yl)propionic acid monohydrate.

Aufarbeitung

  1. stirringstirred at a room temperature for 1 hour
  2. customThe crystals formed
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customdried
  6. customThe crude crystals thus obtained
  7. filtrationthe crystals were collected by filtration
  8. dissolutiondissolved in a saturated sodium bicarbonate aqueous solution
  9. customThe insoluble materials were removed by filtration
  10. customthe filtrate obtained
  11. customThe crystals formed
  12. filtrationwere collected by filtration
  13. washwashed with water
  14. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cbeee661e40c4f60b3642760e47becea
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04694017

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