Sodium Hydroxide → HCID 13565003, compound

HRID 236575Notes

Reaction equation

HRID 236575 reaction equation
[CH3:1][C:2]1[NH:3][C:4]([CH3:42])=[C:5]([C:26]([O:28][CH2:29][CH2:30][N:31]2C(=O)C3=CC=CC=C3C2=O)=[O:27])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][C:18](=O)[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:7]=1[N+:8]([O-:10])=[O:9].O.NN.[OH-].[Na+]>C(O)C>[CH3:1][C:2]1[NH:3][C:4]([CH3:42])=[C:5]([C:26]([O:28][CH2:29][CH2:30][NH2:31])=[O:27])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH2:18][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:7]=1[N+:8]([O-:10])=[O:9]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 70431246HCID 70431246, compound

Product 1

HCID 13565003HCID 13565003, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

14.5 g (26.22 mmol) of β-phthalimido-ethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-benzoyloxyphenyl)-pyridine-5-carboxylate are suspended in 260 ml of ethanol, and 7 ml (140 mmol) of hydrazine hydrate in 20 ml of ethanol are added dropwise, while boiling. The mixture is boiled for 2 hours, cooled and filtered with suction. The resulting solid product is stirred with 200 mmol of 0.5 N sodium hydroxide solution for 30 minutes, filtered off with suction, washed with water and ethanol and dried. 9.5 g of crystals which are red-orange in color and have a melting point of 216° C. are obtained.

Workup

  1. temperaturecooled
  2. filtrationfiltered with suction
  3. filtrationfiltered off with suction
  4. washwashed with water and ethanol
  5. customdried
  6. customare obtained

Sources & evidence

ORD record
ord-1d1294a5fb034960b6e35190b41808a5
Source dataset
uspto-grants-1987_02
Patent number
US04645775

Reaction notes

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