Sodium Hydroxide → HCID 54010487, compound

HRID 1702616Notes

Reaction equation

Cl[C:2]1[N:7]=[C:6](Cl)[N:5]=[C:4]([N:9]=[CH:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:3]=1.[NH2:16][CH:17]1[CH2:22][C:21]([CH3:24])([CH3:23])[NH:20][C:19]([CH3:26])([CH3:25])[CH2:18]1.[OH-:27].[Na+].[NH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36]>C1(C)C=CC=CC=1>[CH2:14]([O:13][C:11]([CH:10]=[N:9][C:4]1[N:5]=[C:6]([NH:16][CH:17]2[CH2:18][C:19]([CH3:26])([CH3:25])[NH:20][C:21]([CH3:24])([CH3:23])[CH2:22]2)[N:7]=[C:2]([NH:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH:36][C:2]2[N:3]=[C:4]([N:9]=[CH:10][C:11]([O:13][CH2:14][CH3:15])=[O:27])[N:5]=[C:6]([NH:16][CH:17]3[CH2:18][C:19]([CH3:26])([CH3:25])[NH:20][C:21]([CH3:24])([CH3:23])[CH2:22]3)[N:7]=2)[N:3]=1)=[O:12])[CH3:15]

Participants

Conditions

Temperature: 40 °C

Procedure

2,4-Dichloro-6-ethoxycarbonylmethyleneamino-1,3,5-triazine (12.5 grams; 0.05 mole), dissolved in toluene (200 mls), is treated with 4-amino-2,2,6,6-tetramethylpiperidine (7.8 grams; 0.05 mole) and powdered sodium hydroxide (2.0 grams; 0.05 mole) and the mixture is stirred at 40° C. for 3 hours. At this point, powdered sodium hydroxide (2.0 grams; 0.05 mole) and hexamethylenediamine (2.9 grams; 0.025 mole) are added and the mixture is heated at reflux for 8 hours. The reaction mixture is filtered and the filtrate is heated under vacuum to remove the solvent. The resulting residue is the desired product.

Workup

temperaturethe mixture is heated
temperatureat reflux for 8 hours
filtrationThe reaction mixture is filtered
temperaturethe filtrate is heated under vacuum
customto remove the solvent

Sources & evidence

ORD record: ord-1779498cd496415e80729287bcdb4fb8
Source dataset: uspto-grants-1982_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04348493

Reaction notes

Loading…