Hydrochloric Acid → 1246210-25-2

HRID 449450Notes

Reaction equation

HRID 449450 reaction equation
CC1(C)OC(=O)[CH:5]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[C:4](=[O:15])[O:3]1.Cl>O>[C:13]([C:9]1([CH2:5][C:4]([OH:15])=[O:3])[CH2:12][CH2:11][CH2:10]1)#[N:14]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 59496759HCID 59496759, compound

Product 1

HCID 553036831246210-25-2

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
100 °C

Procedure

The reaction mixture of 1-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)cyclobutanecarbonitrile (0.32 g, 1.4 mmol) in N,N-dimethylformate (4.0 mL) and water (0.40 mL) was stirred at 100° C. for 2 h. After cooled to r.t., the mixture was diluted with water, adjusted to pH=2 with aqueous HCl, and extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure to afford the crude product which was directly used in next step reaction without further purification.

Workup

  1. temperatureAfter cooled to r.t.
  2. extractionextracted with ethyl acetate (3×20 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-dce65a5a014e4e76a647fecd26aebc7a
Source dataset
uspto-grants-2013_07
Patent number
US08481732B2

Reaction notes

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