Ethanol → Rifaximin

HRID 1747726ノート

反応式

HRID 1747726 の反応式
O.C(O)C.[CH3:5][C@@H:6]1[C@H:40]([OH:41])[C@@H:39]([CH3:42])[C@@H:38]([OH:43])[C@@H:37]([CH3:44])[C@H:36]([O:45][C:46]([CH3:48])=[O:47])[C@H:35]([CH3:49])[C@@H:34]([O:50][CH3:51])[CH:33]=[CH:32][O:31][C@:28]2([CH3:52])[C:29](=[O:30])[C:18]3[C:19]([O:27]2)=[C:20]([CH3:26])[C:21]([OH:25])=[C:22]2[C:23](=[O:24])[C:14](=[CH:15][C:16]4(OC(=O)CO4)[C:17]=32)[NH:13][C:11](=[O:12])[C:10]([CH3:58])=[CH:9][CH:8]=[CH:7]1.[NH2:59][C:60]1[CH:65]=[C:64]([CH3:66])[CH:63]=[CH:62][N:61]=1>CC(C)=O>[CH3:66][C:64]1[CH:63]=[CH:62][N:61]2[C:15]3[C:14]4[NH:13][C:11](=[O:12])[C:10]([CH3:58])=[CH:9][CH:8]=[CH:7][C@H:6]([CH3:5])[C@H:40]([OH:41])[C@@H:39]([CH3:42])[C@@H:38]([OH:43])[C@@H:37]([CH3:44])[C@H:36]([O:45][C:46]([CH3:48])=[O:47])[C@H:35]([CH3:49])[C@@H:34]([O:50][CH3:51])[CH:33]=[CH:32][O:31][C@:28]5([CH3:52])[C:29](=[O:30])[C:18]6=[C:19]([O:27]5)[C:20]([CH3:26])=[C:21]([OH:25])[C:22](=[C:17]6[C:16]=3[N:59]=[C:60]2[CH:65]=1)[C:23]=4[OH:24]

参加物

6

反応物 4

HCID 702EthanolHCID 962WaterHCID 15332-Amino-4-methylpyridineHCID 5280468Rifamycin, 4-O-(carboxymethyl)-1-deoxy-1,4-dihydro-4-hydroxy-1-oxo-, gamma-lactone

生成物 1

HCID 6436173Rifaximin

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

In flask equipped with a mechanic stirrer, 200 ml of demineralized water, 150 ml of ethyl alcohol, 50 ml of acetone, 100 g of Rifamycin O and 43.3 g of 2-amino-4-methylpyridine are loaded in succession at room temperature. After loading, the mixture is kept under stirring at room temperature for 24 hours, then is cooled to 10° C. for 60 minutes. Then the precipitate is filtered and washed by means of a mixture of 100 ml of demineralized water and 100 ml of ethyl alcohol and at least with two washing of 100 ml of demineralized water. The product is dried under vacuum at 70° C. until the water content is between 2.0 and 4.5%.

後処理

  1. customIn flask equipped with a mechanic stirrer
  2. customare loaded in succession at room temperature
  3. temperatureis cooled to 10° C. for 60 minutes
  4. filtrationThen the precipitate is filtered
  5. washwashed by means of a mixture of 100 ml of demineralized water and 100 ml of ethyl alcohol
  6. washat least with two washing of 100 ml of demineralized water
  7. dry with materialThe product is dried under vacuum at 70° C. until the water content

出典と根拠

ORDレコード
ord-4c9e5e709a674d60a49a7343af7aa127
出典データセット
uspto-grants-2015_10
特許番号
US09150590B2

反応ノート

読み込み中…