Diisopropyl Ether → HCID 178467383, compound

HRID 885421Notes

Reaction equation

[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1.[CH2:10]([O:12][C:13](OCC)(OCC)OCC)[CH3:11].C(OC(C)C)(C)C>>[CH2:10]([O:12][C:13]1[NH:1][C:2]2=[N:3][CH:4]=[CH:5][C:6]([CH3:9])=[C:7]2[N:8]=1)[CH3:11]

Participants

Reactant 3

HCID 7914Diisopropyl Ether

HCID 66213Tetraethyl orthocarbonate

HCID 3174954-Methylpyridine-2,3-diamine

Product 1

HCID 178467383HCID 178467383, compoundYield 68%

Conditions

Temperature: 150 °C

Procedure

2,3-Diamino-4-methylpyridine (U.S. Pat. No. 5,332,744; 2.00 g, 16.2 mmol) and tetraethoxymethane (15.0 mL, 71.7 mmol) were mixed, and the mixture was stirred at 150° C. for 2 hr. The mixture was cooled to room temperature, diisopropyl ether (15 mL) was added thereto and the precipitated solid was collected by filtration to give the title compound (1.96 g, 68%).

Workup

temperatureThe mixture was cooled to room temperature
filtrationthe precipitated solid was collected by filtration

Sources & evidence

ORD record: ord-56972f375fe2438eb4fc7f38bd20a52d
Source dataset: uspto-grants-2012_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08242151B2

Reaction notes

Loading…