Sodium Hydroxide → HCID 19004097, compound

HRID 2225366Notes

Reaction equation

HRID 2225366 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][C:25]([O:27]CC)=[O:26])[CH2:20][CH2:19]3)[C:8]=2[CH:30]=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][C:25]([OH:27])=[O:26])[CH2:22][CH2:23]3)[C:8]=2[CH:30]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 19004072HCID 19004072, compound

Product 1

HCID 19004097HCID 19004097, compoundYield 97.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

2N Aqueous sodium hydroxide solution (5 ml) was added to a solution of 2.08 g of ethyl 4-(2-chlorodibenzo[b,f][1,4]thiazepin-11-yl)-1-piperazineacetate in 21 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 yellowish viscous precipitates were extracted with chloroform. The chloroform layer was washed with water, dried and concentrated to give 1.89 g of pale yellow crystals, which were recrystallized from ethanol to give pale yellow crystals, mp 139°-141° C.

Workup

  1. temperatureThe solution was refluxed for 30 min
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in hot water
  4. customThe yellowish viscous precipitates
  5. extractionwere extracted with chloroform
  6. washThe chloroform layer was washed with water
  7. customdried
  8. concentrationconcentrated

Sources & evidence

ORD record
ord-614ed30ecf9844b8b2d8280219fe7105
Source dataset
uspto-grants-1994_09
Patent number
US05344828

Reaction notes

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