Ethyl formate → HCID 14419061, compound

HRID 1110690Notes

Reaction equation

HRID 1110690 reaction equation
[C:1]1([CH2:7][CH2:8][NH:9][CH:10]2[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:20](OCC)=[O:21]>CCCCO.CCCCO.CCCCO.CCCCO.[Ti]>[C:1]1([CH2:7][CH2:8][N:9]([CH:10]2[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]2)[CH:20]=[O:21])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 8025Ethyl formateHCID 13879305HCID 13879305, compound

Product 1

HCID 14419061HCID 14419061, compound

Reagents, catalysts & solvents 1

HCID 521701TetrabutoxytitaniumCatalyst

Procedure

114 g of 4-(N-phenylethylamino)-2,2,6,6-tetramethylpiperidine and 41.3 g of tetrabutyl orthotitanate in 220 ml of ethyl formate were refluxed for 14.5 hours. After the volatile constituents had been distilled off at 140° C./1 mmHg, the solidified residue was recrystallized from petroleum ether. 4-(N-phenylethyl-N-formylamino)-2,2,6,6-tetramethylpiperidine of melting point 86° C. was isolated.

Workup

  1. distillationAfter the volatile constituents had been distilled off at 140° C./1 mmHg
  2. customthe solidified residue was recrystallized from petroleum ether

Sources & evidence

ORD record
ord-5f5fc97cb4f0465ca72961225e1ee1b4
Source dataset
uspto-grants-1990_12
Patent number
US04976889

Reaction notes

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