Phosphoric Acid → HCID 58136555, compound

HRID 877156Notes

Reaction equation

HRID 877156 reaction equation
P(=O)(O)(O)[OH:2].[CH3:6][CH:7]([CH3:16])[CH2:8][CH:9]([S:13][C:14]#[N:15])[C:10](=O)[CH3:11]>O>[CH3:11][C:10]1[NH:15][C:14](=[O:2])[S:13][C:9]=1[CH2:8][CH:7]([CH3:16])[CH3:6]

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 86650854HCID 86650854, compound

Product 1

HCID 58136555HCID 58136555, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
95 °C

Procedure

25 ml of 85% strength phosphoric acid were added to 20.07 g (117.26 mmol) of 5-methyl-2-oxohexan-3-yl thiocyanate, and the mixture was heated to 95° C. over a period of 1 h. At a temperature of 95-100° C., the mixture was stirred for another 0.5 h. After cooling, the reaction mixture was added to 40 ml of water and extracted repeatedly with tert-butyl methyl ether. The combined organic phases were washed with water, dried over sodium sulfate and concentrated on a rotary evaporator. This gave 18.11 g of the target compound, which was reacted further without further purification.

Workup

  1. temperatureAfter cooling
  2. extractionextracted repeatedly with tert-butyl methyl ether
  3. washThe combined organic phases were washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated on a rotary evaporator
  6. customThis gave 18.11 g of the target compound, which was reacted further without further purification

Sources & evidence

ORD record
ord-61240138c4ab45b8a7823e0f63691a02
Source dataset
uspto-grants-2015_03
Patent number
US08987256B2

Reaction notes

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