Sodium Chloride → HCID 59829785, compound

HRID 1947227Notes

Reaction equation

[CH:1]([C:4]1[C:5]([O:23][CH2:24][O:25][CH3:26])=[CH:6][C:7]([O:19][CH2:20][O:21][CH3:22])=[C:8]([C:10]2[N:11]([CH:16]([CH3:18])[CH3:17])[C:12](=[S:15])[NH:13][N:14]=2)[CH:9]=1)([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Cl.[CH3:34][N:35]([CH3:40])[CH2:36][CH2:37][CH2:38]Cl.[Cl-].[Na+]>C(O)C>[CH:1]([C:4]1[C:5]([O:23][CH2:24][O:25][CH3:26])=[CH:6][C:7]([O:19][CH2:20][O:21][CH3:22])=[C:8]([C:10]2[N:11]([CH:16]([CH3:18])[CH3:17])[C:12]([S:15][CH2:38][CH2:37][CH2:36][N:35]([CH3:40])[CH3:34])=[N:13][N:14]=2)[CH:9]=1)([CH3:2])[CH3:3]

Participants

Conditions

Temperature: 100 °C

Procedure

5-(5-isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-isopropyl-2,4-dihydro-[1,2,4]triazol-3-thione (F63-03: 114 mg, 0.3 mmol), potassium carbonate (249 mg, 1.8 mmol) and ethanol (10 mL) were placed in a test tube, and next 3-dimethylaminopropyl chloride hydrochloride (1.49 g, 9.4 mmol) was added. The mixture was stirred at 100° C. for 1 hour. After completing the reaction, the reaction mixture was cooled naturally, mixed with saturated sodium chloride solution and extracted twice with ethyl acetate. The organic layers were combined, washed 4 times with saturated sodium chloride solution, then dried with sodium sulfate and concentrated under reduced pressure.

Workup

customthe reaction
temperaturethe reaction mixture was cooled naturally
extractionextracted twice with ethyl acetate
washwashed 4 times with saturated sodium chloride solution
dry with materialdried with sodium sulfate
concentrationconcentrated under reduced pressure

Sources & evidence

ORD record: ord-1454a5a603484804ba1cf22fba024eff
Source dataset: uspto-grants-2013_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08399464B2

Reaction notes

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