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

HRID 2309251

반응식

HRID 2309251 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric Acid2회HCID 887MethanolHCID 962WaterHCID 27875262-[(4-chlorophenyl)formamido]-3-(1H-indol-3-yl)propanoic acid

생성물 1

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

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbeee661e40c4f60b3642760e47becea
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04694017

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