Dimethylamine → HCID 13726357, compound

HRID 247332Notes

Reaction equation

HRID 247332 reaction equation
Cl[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH2:11][CH3:12])[C:8](=[O:13])[C:7]2[CH:14]=[CH:15][CH:16]=[CH:17][C:6]=2[N:5]1[CH3:18].[CH3:19][NH:20][CH3:21]>C(O)C>[CH3:19][N:20]([CH3:21])[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH2:11][CH3:12])[C:8](=[O:13])[C:7]2[CH:14]=[CH:15][CH:16]=[CH:17][C:6]=2[N:5]1[CH3:18]

Participants

4

Reactant 2

HCID 674DimethylamineHCID 13726307HCID 13726307, compound

Product 1

HCID 13726357HCID 13726357, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 30 g (0.112 mole) of 2-(2-chloroethyl)-4-ethyl-1-methyl-1,2,3,4-tetrahydro-5H-1,4-benzodiazepin-5-one and 10 g (0.224 mole) of dimethylamine in 300 ml of ethanol was heated at 125° C. for 8 hrs and concentrated. The residue was partitioned between chloroform and dilute sodium hydroxide. The chloroform was dried over anhydrous sodium sulfate, concentrated and distilled. Yield of product was 20.5 g (66.5%), b.p. 175°-178°/0.1 mm.

Workup

  1. concentrationconcentrated
  2. customThe residue was partitioned between chloroform and dilute sodium hydroxide
  3. dry with materialThe chloroform was dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. distillationdistilled

Sources & evidence

ORD record
ord-490ac57c6a6d45f8bf08d1b3fb22b80b
Source dataset
uspto-grants-1987_11
Patent number
US04705853

Reaction notes

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