HCID 21242097, compound → HCID 21242102, compound

HRID 622140Notes

Reaction equation

[C:1]1([C:7]2[CH:8]=[C:9]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][O:26]C4CCCCO4)[CH2:20][CH2:19]3)[N:10]3[CH:16]=[CH:15][C:14](=[O:17])[CH:13]=[CH:12][C:11]=23)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(Cl)(Cl)Cl.CO.Cl.C(Cl)Cl>[OH:26][CH2:25][CH2:24][N:21]1[CH2:22][CH2:23][N:18]([C:9]2[N:10]3[CH:16]=[CH:15][C:14](=[O:17])[CH:13]=[CH:12][C:11]3=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH:8]=2)[CH2:19][CH2:20]1

Participants

Conditions

Temperature: 20 °C

Procedure

To a solution of 1-phenyl-3-[4-(2-tetrahydropyranyloxyethyl)-1-piperazinyl]-7H-pyrrolo[1,2-a]azepin-7-one (1.5 g) in chloroform (15 cc) and methanol (15 cc), 11.5M aqueous hydrochloric acid solution (1 cc) is added and the mixture is stirred at a temperature of about 20° C. for 12 hours. The solvents are evaporated off and the residue thereby obtained is dissolved in methylene chloride (50 cc). The solution is washed with 1N aqueous sodium hydroxide solution (25 cc) and twice with distilled water (50 cc in total), dried over anhydrous magnesium sulphate in the presence of decolorizing charcoal, filtered and evaporated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 40° C. 3-[4-(2-Hydroxyethyl)-1-piperazinyl]-1-phenyl-7H-pyrrolo[1,2-a]azepin-7-one (0.28 g) is thereby obtained in the form of a pale yellow oil.

Workup

customThe solvents are evaporated off
customthe residue thereby obtained
washThe solution is washed with 1N aqueous sodium hydroxide solution (25 cc) and twice with distilled water (50 cc in total)
dry with materialdried over anhydrous magnesium sulphate in the presence of decolorizing charcoal
filtrationfiltered
customevaporated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 40° C

Sources & evidence

ORD record: ord-93656e75d350420ba73245a5b9e1f1b1
Source dataset: uspto-grants-1988_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04769366

Reaction notes

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