Hydrochloric Acid → HCID 86753942, compound

HRID 1418902Notes

Reaction equation

HRID 1418902 reaction equation
[Cl:1][C:2]1[C:7]2[C:8](=[O:31])[N:9]3[CH2:30][CH2:29][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[O:17][C:18]([CH2:21][N:22]([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25])=[CH:19][N:20]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.Cl.CCOCC>C(O)C>[ClH:1].[Cl:1][C:2]1[C:7]2[C:8](=[O:31])[N:9]3[CH2:30][CH2:29][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[O:17][C:18]([CH2:21][N:22]([CH2:23][CH2:24][CH3:25])[CH2:26][CH2:27][CH3:28])=[CH:19][N:20]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 18392572HCID 18392572, compound

Product 1

HCID 86753942HCID 86753942, compoundYield 163.4%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.13 g (0.00257 mol) of (S)-8-chloro-1-(5-dipropylaminomethyl-oxazol-2-yl)-12,12a-dihydro-9H,11H-azeto[2,1-c]-imidazo[1,5-a][1,4]benzodiazepin-9-one in 50 ml ethanol were treated at 0° with 0.73 ml (0.00270 mol) of 3.7N ethanolic hydrochloric acid. A suspension was obtained after stirring at 0° for 1/4 hr. It was treated with 50 ml of ether and suction filtered. There was obtained 1.0 g (82%) of (S)-8-chloro-1-(5-dipropylaminomethyl-oxazol-2-yl)-12,12a-dihydro-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepin-9-one hydrochloride (1:1) as white crystals; m.p. 237°-240° (dec.) and [α]D20 =-163.4° (H2O, c=1%).

Workup

  1. customA suspension was obtained
  2. filtrationfiltered

Sources & evidence

ORD record
ord-3c36d92f21bb46e9a4acde5bf8938978
Source dataset
uspto-grants-1999_03
Patent number
US05885986

Reaction notes

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