1,4-Dioxane hydrochloride → Hydrochloric Acid

HRID 2237431Notes

Reaction equation

HRID 2237431 reaction equation
C(OC([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[C:16]([Br:18])[S:17][C:11]=2[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:19].O1CCOCC1>CCOCC>[Br:18][C:16]1[S:17][C:11]2[CH2:10][CH2:9][NH:8][CH2:14][CH2:13][C:12]=2[CH:15]=1.[ClH:19]

Participants

5

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 593025511,1-Dimethylethyl 2-bromo-4,5,7,8-tetrahydro-6H-thieno[2,3-d]azepine-6-carboxylate

Product 2

HCID 313Hydrochloric AcidHCID 115359692-BROMO-5,6,7,8-TETRAHYDRO-4H-THIENO[2,3-D]AZEPINE

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

The product of step g) (0.39 mmol) dissolved in ether (1 ml) was treated with 4 M HCl/dioxane (1 ml). The reaction mixture was stirred for 18 hours at ambient temperature. The resulting precipitate was filtered and washed with anhydrous diethyl ether to give the title compound as its HCl salt. 1H NMR (300 MHz, DMSO) δ 9.40 (s, 2H), 7.05 (s, 1H), 3.14-3.33 (m, 4H), 2.94-3.23 (m, 2H), 2.76-3.06 (m, 2H). MS: ESI (positive): 232, 234 (M+H).

Workup

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with anhydrous diethyl ether

Sources & evidence

ORD record
ord-1284d3a8d0b544cc8440ba1055830255
Source dataset
uspto-grants-2010_05
Patent number
US07718647B2

Reaction notes

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