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Water → HCID 178441399, compound

HRID 2231435
Notes
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Reaction equation

HRID 2231435 reaction equation
C(=O)([O-])[O-].[Ba+2].O.[CH3:7][CH2:8][CH2:9][CH2:10][CH:11]1[C:46](=[O:47])[O:45][CH:44]([CH:48]([CH:50]([OH:58])[CH2:51][CH2:52][CH2:53][NH:54][C:55]([NH2:57])=[NH:56])[CH3:49])[CH:43]([CH3:59])[CH:42]=[C:41]([CH3:60])[CH2:40][CH2:39][CH2:38][CH2:37][CH:36]([OH:61])[CH2:35][CH:34]([OH:62])[CH2:33][CH:32]([OH:63])[CH2:31][CH:30]([OH:64])[CH2:29][CH:28]([OH:65])[CH:27]([O:66][C@H:67]2[O:71][C@H:70]([CH2:72][OH:73])[C@@H:69]([OH:74])[C@@H:68]2[OH:75])[CH:26]=[C:25]([CH3:76])[CH:24]([OH:77])[CH2:23][CH2:22][CH2:21][CH:20]([OH:78])[CH2:19][CH2:18][CH2:17][CH:16]([OH:79])[CH2:15][CH2:14][CH:13]([CH3:80])[CH:12]1[OH:81].S([O-])([O-])(=O)=O.[Cl:87]([OH:91])(=[O:90])(=[O:89])=[O:88]>CO>[CH3:7][CH2:8][CH2:9][CH2:10][CH:11]1[C:46](=[O:47])[O:45][CH:44]([CH:48]([CH:50]([OH:58])[CH2:51][CH2:52][CH2:53][NH:54][C:55]([NH2:57])=[NH:56])[CH3:49])[CH:43]([CH3:59])[CH:42]=[C:41]([CH3:60])[CH2:40][CH2:39][CH2:38][CH2:37][CH:36]([OH:61])[CH2:35][CH:34]([OH:62])[CH2:33][CH:32]([OH:63])[CH2:31][CH:30]([OH:64])[CH2:29][CH:28]([OH:65])[CH:27]([O:66][C@H:67]2[O:71][C@H:70]([CH2:72][OH:73])[C@@H:69]([OH:74])[C@@H:68]2[OH:75])[CH:26]=[C:25]([CH3:76])[CH:24]([OH:77])[CH2:23][CH2:22][CH2:21][CH:20]([OH:78])[CH2:19][CH2:18][CH2:17][CH:16]([OH:79])[CH2:15][CH2:14][CH:13]([CH3:80])[CH:12]1[OH:81].[Cl:87]([O-:91])(=[O:90])(=[O:89])=[O:88]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 10563Barium CarbonateHCID 24247Perchloric AcidHCID 178441404HCID 178441404, compound

Product 1

HCID 178441399HCID 178441399, compoundYield 88.7%

Reagents, catalysts & solvents 1

HCID 887
Methanol
Solvent

Procedure

0.087 g (0.444 millimoles) of barium carbonate is dissolved in 8.87 ml of a 0.1N aqueous perchloric acid solution under slight warming whereupon water is removed in vacuo. The residue is taken up in 10 ml of methanol and added to a suspension of 1.0 g (0.887 millimoles) of primycin sulfate in 80 ml of methanol. The reaction mixture is heated to boiling for 20 minutes under stirring. The primycin perchlorate thus formed remains in the solution and the barium sulfate is precipitated. The hot solution is filtered over Celite and the solid is thoroughly washed on the filter with 10 ml of a 2:1 mixture of acetone and water. Thus 0.94 g of white primycin perchlorate is obtained, yield 88.7%. Mp.: 170°-171° C., /α/D25 =+20°.

Workup

  1. customis removed in vacuo
  2. temperatureThe reaction mixture is heated
  3. customThe primycin perchlorate thus formed remains in the solution and the barium sulfate is precipitated
  4. filtrationThe hot solution is filtered over Celite
  5. washthe solid is thoroughly washed on the
  6. filtrationfilter with 10 ml of a 2:1 mixture of acetone and water

Sources & evidence

ORD record
ord-2a213164d9a64b07b9f1ae7fd86676b9
Source dataset
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04782141

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes