Methylamine → HCID 135965020, compound

HRID 1079344Notes

Reaction equation

HRID 1079344 reaction equation
Cl[C:2]1[CH2:3][S:4][C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=2[CH2:7][N:8]=1.[CH3:13][NH2:14]>C(O)C>[CH3:13][N:14]=[C:2]1[NH:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[S:4][CH2:3]1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 23366675HCID 23366675, compound

Product 1

HCID 135965020HCID 135965020, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

3-Chloro-2,5-dihydro-1,4-benzothiazepine (5 g) and a 33% solution of methylamine in absolute ethanol (150 ml) were heated under reflux for one hour. The mixture was cooled and filtered. Purification of the residue by flash chromatography using ethyl acetate/ethanol (1:1) as eluent gave 3-methylimino-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethanol. Yield 0.51 g (m.p. 278°-280° C.).

Workup

  1. temperatureunder reflux for one hour
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. customPurification of the residue by flash chromatography

Sources & evidence

ORD record
ord-c6c9d944032345cb8aeb74c0b09402c8
Source dataset
uspto-grants-1996_12
Patent number
US05580866

Reaction notes

Loading…