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Hydrogen Bromide → HCID 178441393、化合物

HRID 1493674
ノート
印刷プレビュー

反応式

HRID 1493674 の反応式
C(=O)([O-])[O-].[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.[BrH:88]>>[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].[Br-:88]
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 4

HCID 260Hydrogen BromideHCID 887MethanolHCID 10563Barium CarbonateHCID 178441404HCID 178441404、化合物

生成物 1

HCID 178441393HCID 178441393、化合物収率 87.2%

実験手順

0.087 g (0.444 millimoles) of barium carbonate is dissolved in 1 ml of 48% hydrogen bromide under slight warming. The solvent is removed in vacuo and the residue is rubbed with ether. The barium bromide is filtered and washed with dichloro methane until all the traces of bromine are removed. The yellow color of barium bromide turns into light beige. This salt is dissolved in 10 ml of methanol and the solution is added to a solution of 1.0 g (0.887 millimoles) of primycin sulfate and 80 ml of methanol. The suspension thus obtained is heated to boiling for 20 minutes under stirring. The precipitated barium sulfate is filtered and the filtrate is evaporated in vacuo. The residue is treated with ether and filtered. The solid is washed on the filter first with 10 ml of a 2:1 mixture of acetone and water and later with 10 ml of a dichloro methane. Thus 0.91 g of beige primycin bromide is obtained, yield 87.2%. Mp.: 138° C., /α/D25 =-20°.

後処理

  1. customThe solvent is removed in vacuo
  2. filtrationThe barium bromide is filtered
  3. washwashed with dichloro methane until all the traces of bromine
  4. customare removed
  5. dissolutionThis salt is dissolved in 10 ml of methanol
  6. customThe suspension thus obtained
  7. temperatureis heated
  8. filtrationThe precipitated barium sulfate is filtered
  9. customthe filtrate is evaporated in vacuo
  10. additionThe residue is treated with ether
  11. filtrationfiltered
  12. washThe solid is washed on the
  13. filtrationfilter first with 10 ml of a 2:1 mixture of acetone and water and later with 10 ml of a dichloro methane

出典と根拠

ORDレコード
ord-a5af71727b0f4f769b443f2782e1eb5e
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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