Methanol → HCID 22276508, compound

HRID 1063887Notes

Reaction equation

HRID 1063887 reaction equation
[NH2:1][CH2:2][CH2:3][SH:4].[OH-:5].[Na+].[Br:7][C:8]1[S:12][C:11]([C:13](=[CH2:17])C([O-])=O)=[CH:10][CH:9]=1.[CH3:18]O>>[Br:7][C:8]1[S:12][C:11]([CH:13]2[S:4][CH2:3][CH2:2][NH:1][C:18](=[O:5])[CH2:17]2)=[CH:10][CH:9]=1

Participants

5

Reactant 4

HCID 887Methanol2×HCID 6058CysteamineHCID 14798Sodium HydroxideHCID 86588731HCID 86588731, compound

Product 1

HCID 22276508HCID 22276508, compound

Procedure

To a solution of 2-aminoethanethiol (37.5 g) and sodium hydroxide (15 g) in methanol (500 ml) was added a solution of ethyl 3-(5-bromo-2-thienylacrylate (97.7 g) in methanol (500 ml) under ice-cooling and a nitrogen atmosphere. After being stirred at room temperature for 3 days, the resulting precipitate was collected by filtration and washed with methanol (MeOH) to afford 7-(5-bromo-2-thienyl)perhydro-1,4-thiazepin-5-one (84.6 g) as a solid.

Workup

  1. temperaturecooling
  2. filtrationthe resulting precipitate was collected by filtration
  3. washwashed with methanol (MeOH)

Sources & evidence

ORD record
ord-04612c86799c4eb89b5f2bd0751717e2
Source dataset
uspto-grants-2005_11
Patent number
US06967197B2

Reaction notes

Loading…