Cyanamide → HCID 87441257, compound

HRID 1890781Notes

Reaction equation

HRID 1890781 reaction equation
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([C:13](=[NH:17])[O:14][CH2:15][CH3:16])[CH2:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1.O.OP([O-])(O)=O.[Na+].O.O.O.O.O.O.O.OP([O-])([O-])=O.[Na+].[Na+].[N:39]#[C:40]N>C(#N)C.O>[Cl:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2([C:13](=[N:17][C:40]#[N:39])[O:14][CH2:15][CH3:16])[CH2:10][CH2:11][CH2:12]2)=[CH:7][CH:8]=1

Participants

7

Reactant 4

HCID 9864CyanamideHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 6096963Phosphoric acid, disodium salt, heptahydrateHCID 68407646HCID 68407646, compound

Product 1

HCID 87441257HCID 87441257, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6342AcetonitrileSolvent

Procedure

To a solution of Example 3A (2.5 g, 9.1 mmol) in acetonitrile (7 mL) was added a solution of sodium phosphate monobasic monohydrate (5.0 g, 36.5 mmol), sodium phosphate dibasic heptahydrate (4.9 g, 18.2 mmol), and cyanamide (0.8 g, 18.2 mmol) in water (70.0 mL). The reaction mixture was stirred at room temperature for 72 hours, and then the mixture was extracted with methylene chloride (3×30 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain the titled compound. MS (ESI+) m/z 263 (M+H)+.

Workup

  1. extractionthe mixture was extracted with methylene chloride (3×30 mL)
  2. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-2ce66eb2e14b47b18775aba62916aa89
Source dataset
uspto-grants-2013_08
Patent number
US08507493B2

Reaction notes

Loading…