Phenazepam → HCID 136353534, compound

HRID 1076393Notes

Reaction equation

HRID 1076393 reaction equation
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1.[O:21]1[CH2:26][CH2:25][N:24]([CH:27](OCC)OCC)[CH2:23][CH2:22]1>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[C:9](=[CH:27][N:24]3[CH2:25][CH2:26][O:21][CH2:22][CH2:23]3)[N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1

Participants

3

Reactant 2

HCID 40113PhenazepamHCID 133024324-(Diethoxymethyl)morpholine

Product 1

HCID 136353534HCID 136353534, compound

Conditions

Temperature
140 °C

Procedure

A mixture consisting of 5 gm of 7-bromo-5-(2'-chloro-phenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one and 17 ml of morpholino-diethoxy-methane was heated for 90 minutes at 140°C, while stirring, and the reaction mixture was then allowed to cool. The cool product was admixed with 150 ml of petroleum ether (b.p. 60°-80°C), the mixture was briefly brought to the boiling point, allowed to cool, and the crystalline substance which had separated out was collected by vacuum filtration and recrystallized from isopropanol, yielding the compound named in the heading, which decomposed slowly between 156° and 185°C.

Workup

  1. temperatureto cool
  2. temperatureto cool
  3. customthe crystalline substance which had separated out
  4. filtrationwas collected by vacuum filtration
  5. customrecrystallized from isopropanol
  6. customyielding the compound
  7. customdecomposed slowly between 156° and 185°C.

Sources & evidence

ORD record
ord-de986cc630c8429b80b20b08e0474375
Source dataset
uspto-grants-1976_05
Patent number
US03956492

Reaction notes

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