Deferoxamine → Deferoxamine hydrochloride

HRID 24973ノート

反応式

HRID 24973 の反応式
[CH3:1][C:2]([N:4]([OH:39])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][NH:10][C:11]([CH2:13][CH2:14][C:15]([N:17]([OH:38])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24]([CH2:26][CH2:27][C:28]([N:30]([OH:37])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36])=[O:29])=[O:25])=[O:16])=[O:12])=[O:3].[Cl-:40].[NH4+]>O>[CH3:1][C:2]([N:4]([OH:39])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][NH:10][C:11]([CH2:13][CH2:14][C:15]([N:17]([OH:38])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24]([CH2:26][CH2:27][C:28]([N:30]([OH:37])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36])=[O:29])=[O:25])=[O:16])=[O:12])=[O:3].[ClH:40]

参加物

4

反応物 2

HCID 2973Deferoxamine2 回HCID 25517Ammonium Chloride2 回

生成物 1

HCID 62880Deferoxamine hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Crude deferoxamine B hydrochloride (7.88 kg) containing 5.30 kg deferoxamine B was dissolved in water (362 L). The aqueous solution was then passed through an equal volume of Diaion® SP 207 adsorption resin (Mitsubishi Chemical Corp.) in a 10 liter chromatographic column at a flow rate of 14 L h−1. The eluent contained 5.04 kg deferoxamine. Ammonium chloride was then added in an amount of 5 g L−1 to the eluent with stirring until the ammonium chloride completely dissolved. The solution was then loaded onto a column containing Amberlite® XAD 1180 adsorption resin (132 L) (Rohm & Haas) and driven into the bed with salt water. The column was eluted with 10% acetonitrile-water and then 20% acetonitrile-water at a flow rate of 14 L h−1. The eluent was collected in fractions. The main fraction yielded deferoxamine hydrochloride solution containing 4.53 kg of deferoxamine B. The main fraction was then decolorized over activated carbon (45 g) and Duolite® C 467 (Rohm and Haas) ion exchange resin in H+ form yielding deferoxamine hydrochloride solution containing 4.03 kg of deferoxamine B.

後処理

  1. dissolutioncompletely dissolved
  2. washThe column was eluted with 10% acetonitrile-water
  3. customThe eluent was collected in fractions

出典と根拠

ORDレコード
ord-9bc3edd52ba64cf8b991370d3f7aa2d9
出典データセット
uspto-grants-2005_02
特許番号
US06858414B2

反応ノート

読み込み中…