Réaction #2383794

ord-05cb33579dfe48a98ddf3334eab1d45f

Équation de réaction

O
water
O
water
Nc1ccc2c(c1)CNCCO2
2,3,4,5-tetrahydro-1,4-benzoxazepin-7-ylamine
CSC(=N)c1cccs1.I
2-thiophenecarboximidothioic acid, methyl ester, hydroiodide
N=C(Nc1ccc2c(c1)CNCCO2)c1cccs1
N-(2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-yl)-2-thiophenecarboximidamide

Solvants

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    FiltrationThe solids were collected by filtration
  2. 2
    workup.DISSOLUTIONThe solid was dissolved in hot ethyl acetate
  3. 3
    Filtrationfiltered
  4. 4
    workup.ADDITIONdiluted with hexane
  5. 5
    FiltrationThe solids were collected by filtration (3.13 g, 64%), MS m/Z 274 [M+H]+

Mode opératoire

To 2,3,4,5-tetrahydro-1,4-benzoxazepin-7-ylamine (3.67 g, 18 mmol) in DMF (60 ml) was added 2-thiophenecarboximidothioic acid, methyl ester, hydroiodide (5.52 g, 19 mmol). The mixture was heated to 50° C. for 24 h. The mixture was poured into water (50 ml), then basic water (150 ml) and was allowed to stir for 1 h. The solids were collected by filtration. The solid was dissolved in hot ethyl acetate, filtered, and diluted with hexane. The solids were collected by filtration (3.13 g, 64%), MS m/Z 274 [M+H]+.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06489322B1uspto-grants-2002_12