Dimethylcarbamoyl Chloride → HCID 21450995, compound

HRID 596201Notes

Reaction equation

HRID 596201 reaction equation
[CH2:1]([C:3]1[S:18][C:6]2[NH:7][CH2:8][CH2:9][N:10]=[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=3)[C:5]=2[CH:4]=1)[CH3:2].[CH3:19][N:20]([CH3:24])[C:21]([Cl:23])=[O:22]>N1C=CC=CC=1>[ClH:23].[ClH:23].[CH2:1]([C:3]1[S:18][C:6]2[N:7]([C:21](=[O:22])[N:20]([CH3:24])[CH3:19])[CH2:8][CH2:9][N:10]=[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=3)[C:5]=2[CH:4]=1)[CH3:2]

Participants

4

Reactant 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 136079792HCID 136079792, compound

Product 1

HCID 21450995HCID 21450995, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
60 °C

Procedure

To a suspension of 5.1 g of 7-ethyl-5-(2-pyridyl)-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine in 50 ml of pyridine is added 2.4 g of dimethylcarbamoyl chloride, and stirred for 24 hours at 60° C. Then pyridine is evaporated under reduced pressure. To the residue is added acetone to crystallize. The crude crystals obtained are recrystallized from ethanol to give 7-ethyl-1-dimethylcarbamoyl-5-(2-pyridyl)-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine dihydrochloride, melting at 183°-192° C with decomposition.

Workup

  1. customThen pyridine is evaporated under reduced pressure
  2. additionTo the residue is added acetone
  3. customto crystallize
  4. customThe crude crystals obtained
  5. customare recrystallized from ethanol

Sources & evidence

ORD record
ord-31e00b5c44cc49f4b330a168a43f1afb
Source dataset
uspto-grants-1977_03
Patent number
US04010184

Reaction notes

Loading…