Citric Acid → HCID 86609029, compound

HRID 2104467Notes

Reaction equation

HRID 2104467 reaction equation
[CH3:1][N:2]([CH3:37])[C:3]([C@@H:5]1[CH2:10][C@@H:9]([NH:11][C:12]([C:14]2[S:15][C:16]3[CH2:17][N:18]([CH3:23])[CH2:19][CH2:20][C:21]=3[N:22]=2)=[O:13])[C@@H:8]([NH:24][C:25](=[S:36])[C:26]([NH:28][C:29]2[CH:34]=[CH:33][C:32]([F:35])=[CH:31][N:30]=2)=[O:27])[CH2:7][CH2:6]1)=[O:4].[C:38]([OH:50])(=[O:49])[CH2:39][C:40]([CH2:45][C:46]([OH:48])=[O:47])([C:42]([OH:44])=[O:43])[OH:41]>C(O)C>[OH2:4].[C:38]([OH:50])(=[O:49])[CH2:39][C:40]([CH2:45][C:46]([OH:48])=[O:47])([C:42]([OH:44])=[O:43])[OH:41].[CH3:1][N:2]([CH3:37])[C:3]([C@@H:5]1[CH2:10][C@@H:9]([NH:11][C:12]([C:14]2[S:15][C:16]3[CH2:17][N:18]([CH3:23])[CH2:19][CH2:20][C:21]=3[N:22]=2)=[O:13])[C@@H:8]([NH:24][C:25](=[S:36])[C:26]([NH:28][C:29]2[CH:34]=[CH:33][C:32]([F:35])=[CH:31][N:30]=2)=[O:27])[CH2:7][CH2:6]1)=[O:4]

Participants

4

Reactant 2

HCID 311Citric AcidHCID 59676759HCID 59676759, compound

Product 1

HCID 86609029HCID 86609029, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Conditions

Temperature
60 °C

Procedure

The compound obtained in Example 389 (6.26 g) was suspended in 20% hydrous ethanol (100 mL), and 1M aqueous citric acid (11.4 mL) was added to the suspension. Under stirring at 60° C., 20% hydrous ethanol was gradually added thereto to dissolve the suspension. After filtration with heating, the solution was allowed to cool to room temperature under stirring and then was left to stand for 1 day. The precipitated crystals were collected through filtration and then dried for 2 hours at room temperature under reduced pressure, and the residue was left to stand for 1 day, to thereby yield the title compound (6.95 g).

Workup

  1. dissolutionto dissolve the suspension
  2. filtrationAfter filtration
  3. temperaturewith heating
  4. temperatureto cool to room temperature
  5. stirringunder stirring
  6. waitwas left
  7. filtrationThe precipitated crystals were collected through filtration
  8. customdried for 2 hours at room temperature under reduced pressure
  9. waitthe residue was left
  10. waitto stand for 1 day

Sources & evidence

ORD record
ord-d1e32b03c0bf4d4ca3c00c23a4352795
Source dataset
uspto-grants-2009_08
Patent number
US07576135B2

Reaction notes

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