1,4-Dioxane hydrochloride → HCID 76145144, compound

HRID 1020242Notes

Reaction equation

HRID 1020242 reaction equation
C(OC(=O)[NH:7][C:8]1[S:9][CH:10]=[C:11]([CH2:13][O:14][CH3:15])[N:12]=1)(C)(C)C.[ClH:17].O1CCOCC1>>[ClH:17].[CH3:15][O:14][CH2:13][C:11]1[N:12]=[C:8]([NH2:7])[S:9][CH:10]=1

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 45117857HCID 45117857, compound

Product 1

HCID 76145144HCID 76145144, compound

Procedure

Carbamate IV (Example 5) (254 mg, 1.04 mmol) was stirred with HCl/dioxane (4 M, 15 mL) for 24 hours, the mixture was allowed to warm from 0° C. to ambient temperature over this period. Volatiles were removed under reduced pressure and the residue was azeotroped several times with toluene. 1H NMR (300 MHz, CD3OD) δ 3.37 (s, 3H), 4.34 (s, 2H), 6.82 (s, 1H).

Workup

  1. temperatureto warm from 0° C. to ambient temperature over this period
  2. customVolatiles were removed under reduced pressure
  3. customthe residue was azeotroped several times with toluene

Sources & evidence

ORD record
ord-399604b717de41c4a9e446df1e79cc6d
Source dataset
uspto-grants-2014_05
Patent number
US08716320B2

Reaction notes

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