Sulfuric Acid → HCID 131733641, compound

HRID 1752159Notes

Reaction equation

HRID 1752159 reaction equation
[OH:1][S:2]([OH:5])(=[O:4])=[O:3].[CH2:6]([NH:9][C:10]1[N:15]=[C:14]([NH:16][CH2:17][CH2:18][CH3:19])[N:13]=[C:12](O)[N:11]=1)[CH2:7][CH3:8]>O1CCOCC1>[S:2]([O:5][C:12]1[N:13]=[C:14]([NH:16][CH2:17][CH2:18][CH3:19])[N:15]=[C:10]([NH:9][CH2:6][CH2:7][CH3:8])[N:11]=1)([OH:1])(=[O:4])=[O:3]

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 178456887HCID 178456887, compound

Product 1

HCID 131733641HCID 131733641, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

95% H2SO4 (28 μL, 0.52 mmol) was added to the suspension of 4,6-bis(propylamino)-1,3,5-triazin-2-ol (CLXXVIII) (110 mg, 0.52 mmol) in 1,4-dioxane (2 mL). The mixture was stirred for 30 min at room temperature. The resultant precipitate were filtered, washed with Et2O and dried to afford 4,6-bis(propylamino)-1,3,5-triazin-2-ol hydrogen sulfate (CLXXIX) in quantitative yield. 400 MHz 1H NMR (CD3OD+CF3COOD, ppm) 3.35-3.45 (3.2H, m), 3.22-3.27 (0.8H, m), 1.58-1.70 (4H, m), 0.91-1.0 (6H, m). ESI-MS (m/z): 212 [M+H]+. Major Fragments (M+H) 170, 128, 86.

Workup

  1. filtrationThe resultant precipitate were filtered
  2. washwashed with Et2O
  3. customdried

Sources & evidence

ORD record
ord-56ae9d0b26b34baf93e03ffbd6f0ff32
Source dataset
uspto-grants-2015_10
Patent number
US09162992B2

Reaction notes

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