Sodium Carbonate → HCID 86733389, compound

HRID 1076045Notes

Reaction equation

HRID 1076045 reaction equation
Cl.[NH2:2][CH2:3][C:4]([N:6]([CH2:22][NH:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=1[C:14](=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:5].C(=O)([O-])[O-].[Na+].[Na+]>>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]2[N:6]([CH2:22][NH:23][C:24](=[O:25])[O:26][CH2:27][CH3:28])[C:4](=[O:5])[CH2:3][N:2]=[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:8]=2[CH:9]=1

Participants

3

Reactant 2

HCID 10340Sodium CarbonateHCID 21541592HCID 21541592, compound

Product 1

HCID 86733389HCID 86733389, compound

Procedure

An aqueous solution of 1 g. of 2-amino-N-[(ethoxycarbonylamino)methyl]-2'-benzoyl-4'-chloroacetanilide hydrochloride is made alkaline with 10% sodium carbonate solution. The base precipitated is extracted with methylene chloride. The extracts are dried over sodium sulfate and evaporated. The residue is taken up in ethanol and the solution obtained is boiled under reflux for 10 minutes. The crude product which remains as the residue after evaporation of the solution is crystallized from methanol/water. Ethyl [(7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepin-1-yl)methyl]carbamate of melting point 124°-216° is obtained.

Workup

  1. customThe base precipitated
  2. extractionis extracted with methylene chloride
  3. dry with materialThe extracts are dried over sodium sulfate
  4. customevaporated
  5. customthe solution obtained
  6. temperatureunder reflux for 10 minutes
  7. customafter evaporation of the solution
  8. customis crystallized from methanol/water

Sources & evidence

ORD record
ord-a777c621e25b494491ad4a328c5ffd4d
Source dataset
uspto-grants-1976_05
Patent number
US03954838

Reaction notes

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