Methylamine → HCID 7131960, compound

HRID 1952989Notes

Reaction equation

HRID 1952989 reaction equation
[CH3:1][NH2:2].[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][S:12](Cl)(=[O:14])=[O:13])=[CH:7][CH:6]=1)#[N:4]>O1CCCC1>[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][S:12]([NH:2][CH3:1])(=[O:14])=[O:13])=[CH:7][CH:6]=1)#[N:4]

Participants

4

Procedure

Gaseous methylamine was introduced into a solution of 0.8 g (3.71 mMol) of 4-cyanobenzenemethanesulphonic acid chloride in 20 ml of tetrahydrofuran until a distinctly alkaline reaction was obtained. The mixture was stirred for a further hour at ambient temperature, the excess methylamine together with the solvent was distilled off in vacuo and the residue was triturated with diethylether. The crystals formed were suction filtered and dried. 420 mg (54% of theory) of colourless crystals were obtained, Mp. 151-152° C.

Workup

  1. customwas obtained
  2. distillationthe excess methylamine together with the solvent was distilled off in vacuo
  3. customthe residue was triturated with diethylether
  4. customThe crystals formed
  5. filtrationwere suction filtered
  6. customdried
  7. custom420 mg (54% of theory) of colourless crystals were obtained

Sources & evidence

ORD record
ord-b8c5c73815ad46f4b70fb9be55f25aaa
Source dataset
uspto-grants-2000_09
Patent number
US06114390

Reaction notes

Loading…