Hydrochloric Acid → Zofran

HRID 642923

반응식

HRID 642923 반응식
[CH3:1][C:2]1[N:6]([CH2:7][CH:8]2[C:21](=[O:22])[C:12]3[C:13]4[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=4[N:19]([CH3:20])[C:11]=3[CH2:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1.[ClH:23]>C(O)(C)C.O>[CH3:1][C:2]1[N:6]([CH2:7][CH:8]2[C:21](=[O:22])[C:12]3[C:13]4[C:18]([N:19]([CH3:20])[C:11]=3[CH2:10][CH2:9]2)=[CH:17][CH:16]=[CH:15][CH:14]=4)[CH:5]=[CH:4][N:3]=1.[OH2:22].[OH2:22].[ClH:23]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 4595Ondansetron

생성물 1

HCID 59774Zofran수율 49%

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

The crude ondansetron from Example 4 (190 grams; 0.65 mol) was suspended in a mixture of isopropanol (1.2 L) and water (0.24 L). Concentrated hydrochloric acid (32% (w/w)) was added until the pH of the mixture was about 1-2 (about 70 mL). The solution was heated to reflux temperature for one hour and then cooled to room temperature. The precipitated crystals were collected by filtration, and dried to provide 117 grams (0.32 mol; 49% yield) of crude ondansetron hydrochloride dihydrate. The purity was determined to be about 98-99% by HPLC.

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux temperature for one hour
  3. filtrationThe precipitated crystals were collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-0310217a65cb45f193e82b9f3ceb3ced
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696356B2

연결된 노트

불러오는 중…