Water → HCID 23317237, compound

HRID 1982104Notes

Reaction equation

HRID 1982104 reaction equation
Cl.Cl[CH:3]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:6]=2[N:5]([CH3:22])[CH2:4]1.O.[NH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>>[Cl:21][C:18]1[CH:19]=[CH:20][C:6]2[N:5]([CH3:22])[CH:3]([CH2:4][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)[CH2:10][N:9]=[C:8]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:7]=2[CH:17]=1

Participants

4

Reactant 3

HCID 962WaterHCID 8082PiperidineHCID 12318099HCID 12318099, compound

Product 1

HCID 23317237HCID 23317237, compound

Procedure

100 mg of 3,8-dichloro-1-methyl-6-phenyl-1,2,3,4-tetrahydro-1,5-benzodiazocine hydrochloride is heated in 10 ml piperidine under reflux for 24 hours. For processing the mass was poured into water, extracted with chloroform and the chloroform was subsequently distilled off in a vacuum. The product was recrystallized from ether and there was obtained 7-chloro-1-methyl-2-piperidinomethyl-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepine which also was identical with the same material obtained in Examples 4 and 6 of application Ser. No. 355 986 directly by heating acyldiamines with phosphoroxychloride and subsequent reaction with piperidine; m.p. 143°-145° C.

Workup

  1. temperatureunder reflux for 24 hours
  2. extractionextracted with chloroform
  3. distillationthe chloroform was subsequently distilled off in a vacuum
  4. customThe product was recrystallized from ether

Sources & evidence

ORD record
ord-02d0cf505dbb4b4dbd134b3ee12c4f51
Source dataset
uspto-grants-1986_06
Patent number
US04595531

Reaction notes

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