Hydrochloric Acid → Ractopamine Hydrochloride

HRID 2094238노트

반응식

HRID 2094238 반응식
[CH3:1][CH:2]([NH:12][CH2:13][CH:14]([OH:22])[C:15]1[CH:16]=[CH:17][C:18]([OH:21])=[CH:19][CH:20]=1)[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([OH:11])=[CH:9][CH:10]=1.[ClH:23]>O>[CH3:1][CH:2]([NH:12][CH2:13][CH:14]([OH:22])[C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=1)[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([OH:11])=[CH:9][CH:10]=1.[ClH:23]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 56052Ractopamine

생성물 1

HCID 14010333Ractopamine Hydrochloride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Racemic ractopamine can also be isolated and purified from conveniently available commercial sources. One kilogram of commercially available Paylean® (Elanco) was stirred overnight with 15 L of water. The mass was filtrated, and the filtrate (11.5 L) was evaporated under reduced pressure to a small volume (ca. 1-2 L). Aqueous potassium carbonate was added to raise pH to ca. 10, and the solution was extracted twice with equal volumes of ethyl acetate. The ethyl acetate extracts were combined, evaporated under reduced pressure to ca. 0.5 L, and an equal volume of hexanes added. After standing overnight, crystals of ractopamine free base (6.83 g) were filtrated. This material was crystallized again from ethyl acetate/hexanes to give pure ractopamine free base (6.01 g). HPLC showed 98.5% purity. A sample of ractopamine free base (120 mg) was stirred with 10 ml of deionized water cooled in an ice-water bath, and 2 M aqueous hydrochloric acid (2 ml) was added slowly. After stirring to dissolve the material, the solution was filtered and lyophilised to give ractopamine hydrochloride (125 mg). The mp was 128-135° C., lit (Merck Index) mp 124-129° C. 1H NMR was consistent. HPLC showed 98.0% chemical purity.

후처리

  1. temperaturecooled in an ice-water bath
  2. dissolutionto dissolve the material
  3. filtrationthe solution was filtered

출처 및 근거

ORD 기록
ord-be7eaa62071b427796ad8710a01cae50
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445542B2

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