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Methanol → HCID 178441400、化合物

HRID 1493668
ノート
印刷プレビュー

反応式

HRID 1493668 の反応式
[C:1](=O)([O-:3])[O-:2].[Ba+2].[CH3:6][CH2:7][CH2:8][CH2:9][CH:10]1[C:45](=[O:46])[O:44][CH:43]([CH:47]([CH:49]([OH:57])[CH2:50][CH2:51][CH2:52][NH:53][C:54]([NH2:56])=[NH:55])[CH3:48])[CH:42]([CH3:58])[CH:41]=[C:40]([CH3:59])[CH2:39][CH2:38][CH2:37][CH2:36][CH:35]([OH:60])[CH2:34][CH:33]([OH:61])[CH2:32][CH:31]([OH:62])[CH2:30][CH:29]([OH:63])[CH2:28][CH:27]([OH:64])[CH:26]([O:65][C@H:66]2[O:70][C@H:69]([CH2:71][OH:72])[C@@H:68]([OH:73])[C@@H:67]2[OH:74])[CH:25]=[C:24]([CH3:75])[CH:23]([OH:76])[CH2:22][CH2:21][CH2:20][CH:19]([OH:77])[CH2:18][CH2:17][CH2:16][CH:15]([OH:78])[CH2:14][CH2:13][CH:12]([CH3:79])[CH:11]1[OH:80].S([O-])([O-])(=O)=O.CO>C(O)=O>[CH3:6][CH2:7][CH2:8][CH2:9][CH:10]1[C:45](=[O:46])[O:44][CH:43]([CH:47]([CH:49]([OH:57])[CH2:50][CH2:51][CH2:52][NH:53][C:54]([NH2:56])=[NH:55])[CH3:48])[CH:42]([CH3:58])[CH:41]=[C:40]([CH3:59])[CH2:39][CH2:38][CH2:37][CH2:36][CH:35]([OH:60])[CH2:34][CH:33]([OH:61])[CH2:32][CH:31]([OH:62])[CH2:30][CH:29]([OH:63])[CH2:28][CH:27]([OH:64])[CH:26]([O:65][C@H:66]2[O:70][C@H:69]([CH2:71][OH:72])[C@@H:68]([OH:73])[C@@H:67]2[OH:74])[CH:25]=[C:24]([CH3:75])[CH:23]([OH:76])[CH2:22][CH2:21][CH2:20][CH:19]([OH:77])[CH2:18][CH2:17][CH2:16][CH:15]([OH:78])[CH2:14][CH2:13][CH:12]([CH3:79])[CH:11]1[OH:80].[CH:1]([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 10563Barium CarbonateHCID 178441404HCID 178441404、化合物

生成物 1

HCID 178441400HCID 178441400、化合物収率 191.6%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

0.088 g (0.446 millimole) of barium carbonate are heated to boiling in 5 ml of formic acid until a clear solution is obtained. The colorless solution is evaporated to dryness in vacuo. The residue is dissolved in 10 ml of methanol and the solution thus obtained is added to a suspension of 1.0 g (0.887 millimole) of primycin sulfate and 70 ml of methanol. The reaction mixture is heated to boiling for 10 minutes under constant stirring. The precipitated barium sulfate is filtered hot through a Celite filtration auxiliary agent. The filtrate is evaporated in vacuo and the solid residue is treated with ether. The white powdery product is washed with 20 ml of a 2:1 mixture of acetone and water and thereafter with anhydrous ether. Thus 0.96 g of primycin formate is obtained, yield 94.8%. Mp.: 162°-164° C., /α/D25 =+31.9°. (in a 2:2:1 mixture of n-butanol, ethanol and water, c=0.1%)

後処理

  1. customis obtained
  2. customThe colorless solution is evaporated to dryness in vacuo
  3. dissolutionThe residue is dissolved in 10 ml of methanol
  4. customthe solution thus obtained
  5. temperatureThe reaction mixture is heated
  6. filtrationThe precipitated barium sulfate is filtered hot through a Celite filtration auxiliary agent
  7. customThe filtrate is evaporated in vacuo
  8. additionthe solid residue is treated with ether
  9. washThe white powdery product is washed with 20 ml of a 2:1 mixture of acetone and water

出典と根拠

ORDレコード
ord-6e0326e9bace466d943079d6311033f3
出典データセット
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05023242

反応ノート

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