Sodium Bicarbonate → HCID 12774374, compound

HRID 652098Notes

Reaction equation

HRID 652098 reaction equation
[CH3:1][N:2]1[C:6]([NH:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[CH:13]=2)=[N:5][C:4]([CH:25]=[N:26]O)=[N:3]1.C(=O)(O)[O-].[Na+]>C(OC(=O)C)(=O)C>[CH3:1][N:2]1[C:6]([NH:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][N:19]3[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]3)[CH:13]=2)=[N:5][C:4]([C:25]#[N:26])=[N:3]1

Participants

4

Reactant 2

HCID 516892Sodium BicarbonateHCID 136393671HCID 136393671, compound

Product 1

HCID 12774374HCID 12774374, compoundYield 42%

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

A solution of 1-methyl-5-[[3-[3-(1-piperidinylmethyl)phenoxy]propyl]amino]-1H-1,2,4-triazole-3-carboxaldehyde oxime (0.75 g) in acetic anhydride (4 ml) was heated at 100° for 10 hours. The mixture was poured onto aqueous sodium bicarbonate and extracted with toluene. The extract was dried (Na2SO4), filtered, and evaporated to give a solid, which was crystallized from diethyl ether and petroleum ether (b.p. 60°-80°) to give the title compound (0.3 g) as a white powder, m.p. 66°-7°.

Workup

  1. extractionextracted with toluene
  2. dry with materialThe extract was dried (Na2SO4)
  3. filtrationfiltered
  4. customevaporated
  5. customto give a solid, which
  6. customwas crystallized from diethyl ether and petroleum ether (b.p. 60°-80°)

Sources & evidence

ORD record
ord-ea72ca16df6d44a5be1f7ecaf942d09a
Source dataset
uspto-grants-1987_06
Patent number
US04670448

Reaction notes

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