Methylamine → HCID 13175695, compound

HRID 1981973Notes

Reaction equation

HRID 1981973 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][CH2:13]Cl)[CH:10]([CH2:15]Cl)[CH2:9][N:8]=[C:7]([C:17]3[O:18][CH:19]=[CH:20][CH:21]=3)[C:6]=2[CH:22]=1.[CH3:23][NH2:24]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH2:12][CH2:13][N:24]([CH3:23])[CH2:15][CH:10]3[CH2:9][N:8]=[C:7]([C:17]3[O:18][CH:19]=[CH:20][CH:21]=3)[C:6]=2[CH:22]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 13175737HCID 13175737, compound

Product 1

HCID 13175695HCID 13175695, compoundYield 45.3%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1 g of 7-chloro-1-(β-chloroethyl)-2-chloromethyl-5-(2-furyl)-2,3-dihydro-1H-1,4-benzodiazepine in 40 ml of methanol is left to react with 0.8 g of methylamine at 50° C. for 3 hours. The reaction mixture is then worked up as described in Example 7. On purification by chromatography, the fractions containing the more highly polar title compound are separated off. 0.4 g of 1,2,3,4,4a,5-hexahydro-9-chloro-3-methyl-7-(2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine is obtained therefrom.

Workup

  1. customOn purification by chromatography
  2. additionthe fractions containing the more highly polar title compound
  3. customare separated off

Sources & evidence

ORD record
ord-332506155c254eeab1ee8e65a2e61c4c
Source dataset
uspto-grants-1986_06
Patent number
US04594436

Reaction notes

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