Water → Ceftiofur

HRID 863651

반응식

HRID 863651 반응식
[CH3:1][O:2]/[N:3]=[C:4](\[C:11]([NH:13][C@@H:14]1[C:17](=[O:18])[N:16]2[C:19]([C:32]([OH:34])=[O:33])=[C:20]([CH2:23][S:24][C:25]([C:27]3[O:31][CH:30]=[CH:29][CH:28]=3)=[O:26])[CH2:21][S:22][C@H:15]12)=[O:12])/[C:5]1[N:9]=[C:8]([NH2:10])[S:7][CH:6]=1.Cl.O>O1CCCC1>[CH3:1][O:2]/[N:3]=[C:4](\[C:11]([NH:13][C@@H:14]1[C:17](=[O:18])[N:16]2[C:19]([C:32]([OH:34])=[O:33])=[C:20]([CH2:23][S:24][C:25]([C:27]3[O:31][CH:30]=[CH:29][CH:28]=3)=[O:26])[CH2:21][S:22][C@H:15]12)=[O:12])/[C:5]1[N:9]=[C:8]([NH2:10])[S:7][CH:6]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 9937686Ceftiofur Hydrochloride

생성물 1

HCID 6328657Ceftiofur수율 84.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Ceftiofur hydrochloride (17.1 g) is slurried for at least one hour at room temperature with 70 ml of tetrahydrofuran and 5.1 ml of water. To this slurry are added 8.6 g of PVP resin followed by 60 ml of tetrahydrofuran. After stirring for 45 minutes this slurry is filtered. The PVP resin is washed with two 31 ml portions of tetrahydrofuran. The filtrate is then added slowly over a period of about one hour to 515 ml of water at 45°-55° C. This slurry is stirred at 45°-55° C. for 30 minutes and filtered immediately at the end of the addition. The solids are washed with 70 ml of water and dried at 50° C. to give 13.5 g of crystalline ceftiofur free acid.

후처리

  1. additionTo this slurry are added 8.6 g of PVP resin
  2. filtrationis filtered
  3. washThe PVP resin is washed with two 31 ml portions of tetrahydrofuran
  4. additionThe filtrate is then added slowly over a period of about one hour to 515 ml of water at 45°-55° C
  5. stirringThis slurry is stirred at 45°-55° C. for 30 minutes
  6. filtrationfiltered immediately at the end of the addition
  7. washThe solids are washed with 70 ml of water
  8. customdried at 50° C.

출처 및 근거

ORD 기록
ord-294a28bd957e460ab232035f87867f3f
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05721359

연결된 노트

불러오는 중…