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Oxalic Acid → HCID 178441403、化合物

HRID 2231434
ノート
印刷プレビュー

反応式

HRID 2231434 の反応式
C(=O)([O-])[O-].[Ba+2].[C:6]([OH:11])(=[O:10])[C:7]([OH:9])=[O:8].[CH3:12][CH2:13][CH2:14][CH2:15][CH:16]1[C:51](=[O:52])[O:50][CH:49]([CH:53]([CH:55]([OH:63])[CH2:56][CH2:57][CH2:58][NH:59][C:60]([NH2:62])=[NH:61])[CH3:54])[CH:48]([CH3:64])[CH:47]=[C:46]([CH3:65])[CH2:45][CH2:44][CH2:43][CH2:42][CH:41]([OH:66])[CH2:40][CH:39]([OH:67])[CH2:38][CH:37]([OH:68])[CH2:36][CH:35]([OH:69])[CH2:34][CH:33]([OH:70])[CH:32]([O:71][C@H:72]2[O:76][C@H:75]([CH2:77][OH:78])[C@@H:74]([OH:79])[C@@H:73]2[OH:80])[CH:31]=[C:30]([CH3:81])[CH:29]([OH:82])[CH2:28][CH2:27][CH2:26][CH:25]([OH:83])[CH2:24][CH2:23][CH2:22][CH:21]([OH:84])[CH2:20][CH2:19][CH:18]([CH3:85])[CH:17]1[OH:86].S([O-])([O-])(=O)=O>CO>[CH3:12][CH2:13][CH2:14][CH2:15][CH:16]1[C:51](=[O:52])[O:50][CH:49]([CH:53]([CH:55]([OH:63])[CH2:56][CH2:57][CH2:58][NH:59][C:60]([NH2:62])=[NH:61])[CH3:54])[CH:48]([CH3:64])[CH:47]=[C:46]([CH3:65])[CH2:45][CH2:44][CH2:43][CH2:42][CH:41]([OH:66])[CH2:40][CH:39]([OH:67])[CH2:38][CH:37]([OH:68])[CH2:36][CH:35]([OH:69])[CH2:34][CH:33]([OH:70])[CH:32]([O:71][C@H:72]2[O:76][C@H:75]([CH2:77][OH:78])[C@@H:74]([OH:79])[C@@H:73]2[OH:80])[CH:31]=[C:30]([CH3:81])[CH:29]([OH:82])[CH2:28][CH2:27][CH2:26][CH:25]([OH:83])[CH2:24][CH2:23][CH2:22][CH:21]([OH:84])[CH2:20][CH2:19][CH:18]([CH3:85])[CH:17]1[OH:86].[C:6]([O-:11])(=[O:10])[C:7]([O-:9])=[O:8]
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 971Oxalic AcidHCID 10563Barium CarbonateHCID 178441404HCID 178441404、化合物

生成物 1

HCID 178441403HCID 178441403、化合物収率 179.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.087 g (0.444 millimoles) of barium carbonate are suspended in 15 ml of mthanol whereupon 0.04 g (0.444 millimoles) of oxalic acid are added. The suspension thus obtained is heated to boiling until all the solid is dissolved (about 10 minutes). The solvent is removed in vacuo. The residue is added to a solution of 1.0 g (0.887 millimoles) of primycin sulfate and 80 ml of methanol and the reaction mixture is heated to boiling for 20 minutes under constant stirring. The precipitated barium sulfate is filtered hot over Celite. The filtrate is evaporated in vacuo. The solid residue is treated with ether and filtered. The solid is washed on the filter with a 2:1 mixture of acetone and water. Thus 0.93 g of white primycin oxalate is obtained, yield 92.2%. Mp.: 186°-187° C., /α/D25 =+40°.

後処理

  1. additionare added
  2. customThe suspension thus obtained
  3. temperatureis heated
  4. dissolutionis dissolved (about 10 minutes)
  5. customThe solvent is removed in vacuo
  6. temperaturethe reaction mixture is heated
  7. filtrationThe precipitated barium sulfate is filtered hot over Celite
  8. customThe filtrate is evaporated in vacuo
  9. additionThe solid residue is treated with ether
  10. filtrationfiltered
  11. washThe solid is washed on the
  12. filtrationfilter with a 2:1 mixture of acetone and water

出典と根拠

ORDレコード
ord-8a943763963d446bb305abcf60f45e8d
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04782141

反応ノート

読み込み中…

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