Sodium Hydroxide → HCID 19004077, compound
Reaction equation
[OH-].[Na+].[Cl:3][C:4]1[CH:5]=[CH:6][C:7]2[S:13][C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[N:10]=[C:9]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][C:26]([O:28]CC)=[O:27])[CH2:20][CH2:19]3)[C:8]=2[CH:31]=1>CO>[Cl:3][C:4]1[CH:5]=[CH:6][C:7]2[S:13][C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[N:10]=[C:9]([N:18]3[CH2:19][CH2:20][N:21]([CH2:24][CH2:25][C:26]([OH:28])=[O:27])[CH2:22][CH2:23]3)[C:8]=2[CH:31]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
2N Aqueous sodium hydroxide solution (5 ml) was added to a solution of 2.15 g of ethyl 4-(2-chlorodibenzo[b,f][1,4]thiazepin-11-yl)-1-piperazinepropionate in 22 ml of methanol. The solution was refluxed for 30 min and then concentrated. The residue was dissolved in hot water and the solution was neutralized with 0.5N hydrochloric acid. The precipitates were collected by filtration to give 1.84 g of pale yellow crystals, which were recrystallized from aqueous ethanol to give pale yellow crystals, mp 120°-121° C.
Workup
- temperatureThe solution was refluxed for 30 min
- concentrationconcentrated
- dissolutionThe residue was dissolved in hot water
- filtrationThe precipitates were collected by filtration
Sources & evidence
- ORD record
- ord-8092346cb9944302b0362a74650de7a8
- Source dataset
- uspto-grants-1994_09
- Patent number
- US05344828
Reaction notes
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