Hydrochloric Acid → Zofran

HRID 642923

反応式

HRID 642923 の反応式
[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]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 4595Ondansetron

生成物 1

HCID 59774Zofran収率 49%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0310217a65cb45f193e82b9f3ceb3ced
出典データセット
uspto-grants-2010_04
特許番号
US07696356B2

関連ノート

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