Hydrochloric Acid → Amphotericin B Calcium Succinic Acid

HRID 973087

反応式

HRID 973087 の反応式
[CH3:1][C@@H:2]1[C@@H:41]([OH:42])[C@@H:40]([CH3:43])[C@H:39]([CH3:44])[O:38][C:36](=[O:37])[CH2:35][C@H:34]([OH:45])[CH2:33][C@H:32]([OH:46])[CH2:31][CH2:30][C@@H:29]([OH:47])[C@H:28]([OH:48])[CH2:27][C@H:26]([OH:49])[CH2:25][C@@:23]2([OH:50])[O:24][C@H:19]([C@H:20]([C:52]([OH:54])=[O:53])[C@@H:21]([OH:51])[CH2:22]2)[CH2:18][C@@H:17]([O:55][C@@H:56]2[O:61][C@H:60]([CH3:62])[C@@H:59]([OH:63])[C@H:58]([NH2:64])[C@@H:57]2[OH:65])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=[CH:3]1.[Cl-].[Cl-].[Ca+2:68].Cl.[C:70]([OH:77])(=[O:76])[CH2:71][CH2:72][C:73]([OH:75])=[O:74]>CO>[CH3:1][C@@H:2]1[C@@H:41]([OH:42])[C@@H:40]([CH3:43])[C@H:39]([CH3:44])[O:38][C:36](=[O:37])[CH2:35][C@H:34]([OH:45])[CH2:33][C@H:32]([OH:46])[CH2:31][CH2:30][C@@H:29]([OH:47])[C@H:28]([OH:48])[CH2:27][C@H:26]([OH:49])[CH2:25][C@@:23]2([OH:50])[O:24][C@H:19]([C@H:20]([C:52]([OH:54])=[O:53])[C@@H:21]([OH:51])[CH2:22]2)[CH2:18][C@@H:17]([O:55][C@@H:56]2[O:61][C@H:60]([CH3:62])[C@@H:59]([OH:63])[C@H:58]([NH2:64])[C@@H:57]2[OH:65])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=[CH:3]1.[Ca:68].[C:70]([OH:77])(=[O:76])[CH2:71][CH2:72][C:73]([OH:75])=[O:74]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1110Succinic AcidHCID 5280965Amphotericin BHCID 5284359Calcium Chloride

生成物 1

HCID 86735085Amphotericin B Calcium Succinic Acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

10.66 g amphotericin B (938γ/mg of activity-equivalent to 10 g of chemical activity) suspended in 2.5 liters of anhydrous methanol containing 11.1 ml of 5% CaCl2 in methanol (equivalent to 200 mg Ca ion) is solubilized by means of 1.8 ml of 5.8 N HCl (pH 3.9). To the resulting solution are added 100 ml of methanol containing 10 g of reagent grade succinic acid to form a mixture of pH 3.2. The pH of the mixture is adjusted to about 7 by the addition of 7.7 ml concentrated NH 4 OH. The mixture is then heated to 45°-50° C and slurried for one hour and thereafter is cooled to room temperature, filtered and the wet cake dried overnight under vacuum at 45° C to yield 9.1 g of crystalline complex.

後処理

  1. customto form
  2. additiona mixture of pH 3.2
  3. additionThe pH of the mixture is adjusted to about 7 by the addition of 7.7 ml
  4. concentrationconcentrated NH 4 OH
  5. temperatureThe mixture is then heated to 45°-50° C
  6. filtrationfiltered
  7. customthe wet cake dried overnight under vacuum at 45° C

出典と根拠

ORDレコード
ord-a4aa26d66a4843c393197a43c5e29653
出典データセット
uspto-grants-1977_10
特許番号
US04054734

関連ノート

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