Sodium Hydroxide → HCID 178524926, compound

HRID 872930Notes

Reaction equation

HRID 872930 reaction equation
[N:1]1[NH:2][C:3]([C:10]([O:12]CC)=[O:11])=[C:4]2[CH2:9][O:8][CH2:7][CH2:6][C:5]=12.[OH-].[Na+]>CO>[N:1]1[NH:2][C:3]([C:10]([OH:12])=[O:11])=[C:4]2[CH2:9][O:8][CH2:7][CH2:6][C:5]=12

Participants

4

Reactant 2

HCID 14798Sodium Hydroxide2×HCID 178470413HCID 178470413, compound

Product 1

HCID 178524926HCID 178524926, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
0 °C

Procedure

Ethyl 2,4,6,7-tetrahydropyrano[4,3-c]pyrazole-3-carboxylate (0.97 g, 4.94 mmol) was dissolved in methanol (20 ml) and cooled to 0° C. with an ice bath. Sodium hydroxide 2 M solution (4.94 ml, 9.89 mmol) was added and the mixture was allowed to cool to RT with stirring. The mixture was stirred for 26 h during which additional 7 ml of sodium hydroxide 2 M solution was added. The solvent was evaporated and the pH adjusted to 2 with 1 M HCl. The formed precipitate was filtered and washed with water. The white solid was dried with vacuum at 40° C. 1H-NMR (400 MHz; d6-DMSO): δ 2.69 (t, 2H), 3.81 (t, 2H), 4.68 (s, 2H), 13.09 (bs, 1H).

Workup

  1. temperatureto cool to RT
  2. additionwas added
  3. customThe solvent was evaporated
  4. filtrationThe formed precipitate was filtered
  5. washwashed with water
  6. customThe white solid was dried with vacuum at 40° C

Sources & evidence

ORD record
ord-7f0a2818c1b84f8b9537a5e38e591a1a
Source dataset
uspto-grants-2015_03
Patent number
US08975254B2

Reaction notes

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