Ammonium Chloride → HCID 23325186, compound

HRID 1380487Notes

Reaction equation

HRID 1380487 reaction equation
[Na].C[Si](C)(C)[C:4]#[C:5][CH:6]([N:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10].[Cl-].[NH4+]>CO>[CH:14](=[N:13][CH:6]([C:5]#[CH:4])[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 13780253Methyl 4-[(phenylmethylene)amino]-6-(trimethylsilyl)-5-hexynoate

Product 1

HCID 23325186HCID 23325186, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

0.0764 g of sodium was dissolved in 5 ml of methanol. The solution was added at room temperature to a solution of 1.0 g of 3A in 2 ml of dry methanol. The mixture was stirred at room temperature for 4 hours, then 0.1765 g of ammonium chloride was added and the mixture was stirred for 15 minutes. Then the methanol was evaporated, the residue was triturated with ether and the solid phase was filtered off. The solvent was evaporated from the filtrate and the residue was distilled to give 4, b.p.: 170° C. (0.07 Torr).

Workup

  1. stirringthe mixture was stirred for 15 minutes
  2. customThen the methanol was evaporated
  3. customthe residue was triturated with ether
  4. filtrationthe solid phase was filtered off
  5. customThe solvent was evaporated from the filtrate
  6. distillationthe residue was distilled
  7. customto give 4, b.p.: 170° C. (0.07 Torr)

Sources & evidence

ORD record
ord-694019a6c8ad45ccb28cbe5e11874e9f
Source dataset
uspto-grants-1986_04
Patent number
US04582529

Reaction notes

Loading…