Dimethylamine → HCID 21271492, compound

HRID 247311Notes

Reaction equation

HRID 247311 reaction equation
[Cl:1][CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[O:12])[C:7]2[CH:13]=[CH:14][CH:15]=[N:16][C:6]=2[S:5]1.[CH3:17][NH:18][CH3:19]>>[ClH:1].[CH3:17][N:18]([CH3:19])[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[O:12])[C:7]2[CH:13]=[CH:14][CH:15]=[N:16][C:6]=2[S:5]1

Participants

3

Procedure

A solution of 1.5 g (0.0058 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one in 20 ml of dimethylamine was stirred at 25° C. in a sealed container for 72 hr. The excess dimethylamine was allowed to evaporate and the residue was partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue, the free base of the title compound, was dissolved in isopropyl alcohol and reacted with hydrogen chloride. The resulting hydrochloride salt weighed 1.5 g (77%), m.p. >250° C.

Workup

  1. customto evaporate
  2. customthe residue was partitioned between chloroform and dilute sodium hydroxide
  3. concentrationThe chloroform layer was concentrated
  4. dissolutionthe residue, the free base of the title compound, was dissolved in isopropyl alcohol
  5. customreacted with hydrogen chloride

Sources & evidence

ORD record
ord-2428564e44794ef8a443f0c1fd59e557
Source dataset
uspto-grants-1987_11
Patent number
US04705853

Reaction notes

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