2,2-Dimethoxy-1-methylethylamine → HCID 178500500, compound

HRID 1415601Notes

Reaction equation

HRID 1415601 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=S)[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)[C:6]=2[CH:19]=1.[CH3:20][O:21][CH:22]([O:26][CH3:27])[CH:23]([NH2:25])[CH3:24]>C(O)CCC>[CH3:20][O:21][CH:22]([O:26][CH3:27])[CH:23]([NH:25][C:10]1[CH2:9][N:8]=[C:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[C:6]2[CH:19]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[N:11]=1)[CH3:24]

Participants

4

Reactant 2

HCID 936582,2-Dimethoxy-1-methylethylamineHCID 212659987-chloro-5-(2-pyridyl)-3H-1,4-benzodiazepine-2(1H)-thione

Product 1

HCID 178500500HCID 178500500, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent2×

Procedure

A solution of 7-chloro-1,3-dihydro-5-(2-pyridyl)-1,4-benzodiazepin-2-thione in butanol solution is refluxed with excess α-aminopropionaldehyde dimethyl acetal. After cooling excess butanol is removed by vacuum distillation and the residue is crystallized from ethyl acetate-hexane to give 2-[[7-chloro-5-(2-pyridyl)-3H-1,4-benzodiazepin-2-yl]amino]propionaldehyde dimethyl acetal.

Workup

  1. customis removed by vacuum distillation
  2. customthe residue is crystallized from ethyl acetate-hexane

Sources & evidence

ORD record
ord-56679135c6384966a2d4f5a80673c4c2
Source dataset
uspto-grants-1977_01
Patent number
US04005099

Reaction notes

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