Sodium Carbonate → HCID 178475053, compound

HRID 1683939Notes

Reaction equation

HRID 1683939 reaction equation
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[Na+].[Na+].[C:10]([NH:13][C@H:14]1[C@H:22]([C@@H:23]([C@@H:25]([CH2:27][OH:28])[OH:26])[OH:24])[O:21][C:17]([C:18]([OH:20])=[O:19])=[CH:16][C@@H:15]1[NH:29][C:30]#[N:31])(=[O:12])[CH3:11]>CO>[C:10]([NH:13][C@H:14]1[C@H:22]([C@@H:23]([C@@H:25]([CH2:27][OH:28])[OH:26])[OH:24])[O:21][C:17]([C:18]([OH:20])=[O:19])=[CH:16][C@@H:15]1[NH:29][C:30]([NH2:31])=[N:2][OH:3])(=[O:12])[CH3:11]

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 9995821HCID 9995821, compound

Product 1

HCID 178475053HCID 178475053, compoundYield 32.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
21 °C

Procedure

Hydroxylamine hydrochloride (1.1 g, 15.85 mmol)(dried under vacuum over P2O5) was dissolved in dried (over 3 A mol. sieves) methanol (20 ml) and sodium carbonate (0.835 g, 7.9 mmol) was added. This was stirred at 21° C. under N2 for 15 min., then solid was filtered off. To the filtrate was then added the product of Example 1, step (i) (500 mg, 1.585 mmol) and stirring under N2 at 21° C. continued for 16 hr. White solid was filtered off, air dried, then dried under high vacuum to give the title compound (Yield, 180 mg).

Workup

  1. customin dried (over 3 A mol
  2. filtrationsolid was filtered off
  3. stirringstirring under N2 at 21° C.
  4. waitcontinued for 16 hr
  5. filtrationWhite solid was filtered off
  6. customair dried
  7. customdried under high vacuum

Sources & evidence

ORD record
ord-960aba67ac4e4d4780cd3cd5cf5d0661
Source dataset
uspto-grants-1997_06
Patent number
US05639786

Reaction notes

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