Sodium Hydroxide → HCID 178479084, compound

HRID 2292830Notes

Reaction equation

HRID 2292830 reaction equation
Cl.Cl.[Cl:3][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[C:6]([Cl:11])[C:5]=1[N:12]=[C:13]1[NH:17][CH2:16][CH2:15][NH:14]1.[OH-].[Na+]>O>[ClH:3].[Cl:3][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[C:6]([Cl:11])[C:5]=1[N:12]=[C:13]1[NH:14][CH2:15][CH2:16][NH:17]1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 178478663HCID 178478663, compound

Product 1

HCID 178479084HCID 178479084, compoundYield 173.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
5 °C

Procedure

A 5-L, 3-neck, round bottom flask equipped with a mechanical stirrer and a thermometer was charged with (4) (150 g, 0.47 mol) and water (5 L). The pH of the suspension was adjusted to 6.5 by adding 5M aqueous sodium hydroxide dropwise, and the resulting suspension was cooled to 5° C. for 2 hours. The off-white solid was collected by filtration, washed with water (2 L) and t-butyl methyl ether (1 L), and dried for 24 hours at 60° C. and 20 mm Hg to provide 115 g (87%) of (5).

Workup

  1. filtrationThe off-white solid was collected by filtration
  2. washwashed with water (2 L) and t-butyl methyl ether (1 L)
  3. customdried for 24 hours at 60° C.

Sources & evidence

ORD record
ord-f6678ff2cb0c4d4a9c3eccde023a39cd
Source dataset
uspto-grants-1997_11
Patent number
US05684156

Reaction notes

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