Sodium Hydroxide → HCID 69955891, compound

HRID 1978919Notes

Reaction equation

HRID 1978919 reaction equation
[CH3:1][C:2]1[N:11]([N:12]2[C:24](=[O:25])[C:22]3[C:23]4[N:15]([C:16]([N+:26]([O-])=O)=[CH:17][C:18]=4[CH2:19][CH2:20][CH:21]=3)[C:14]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:13]2)[C:10](=[O:35])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH-].[Na+]>[Cl-].[Cl-].[Cl-].[Ti+3].C(O)(=O)C>[NH2:26][C:16]1[N:15]2[C:14]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:13][N:12]([N:11]3[C:10](=[O:35])[C:9]4[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=4)[N:3]=[C:2]3[CH3:1])[C:24](=[O:25])[C:22]3=[CH:21][CH2:20][CH2:19][C:18]([CH:17]=1)=[C:23]23

Participants

5

Reactant 2

HCID 14798Sodium HydroxideHCID 69954865HCID 69954865, compound

Product 1

HCID 69955891HCID 69955891, compound

Reagents, catalysts & solvents 2

HCID 10313229titanium(III) trichlorideCatalystHCID 176Acetic AcidSolvent

Procedure

An alternative process consists in using titanium trichloride as reducing agent. Thus, in a reactor under nitrogen, protected from moisture and equipped with a magnetic stirrer, 5.0 g (10.7 minol) of the product of Example 20 are introduced into 42.8 ml of acetic acid. 64 mmol of TiCl3 (in 30% solution in 2N HCl) are added dropwise and the mixture is kept stirring for 30 min. It is then alcalinized with sodium hydroxide to a pH of 9, the medium being cooled by adding ice.

Workup

  1. customThus, in a reactor under nitrogen, protected from moisture
  2. customequipped with a magnetic stirrer
  3. temperaturethe medium being cooled
  4. additionby adding ice

Sources & evidence

ORD record
ord-898544c651164c6db8b8ce7fa52f70eb
Source dataset
uspto-grants-2001_05
Patent number
US06239130B1

Reaction notes

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