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Water → HCID 21538544, compound

HRID 1076895
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Reaction equation

HRID 1076895 reaction equation
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:20]=[CH:19][C:18]2[S:17][C:16]3[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24]Cl)=[CH:14][CH:15]=3)[CH2:10][C:9]=2[CH:8]=1)=[O:6].[I-].[K+].[NH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1.O>C(Cl)(Cl)Cl>[OH2:6].[ClH:1].[ClH:1].[N:29]1([CH2:2][CH2:3][CH2:4][C:5]([C:7]2[CH:20]=[CH:19][C:18]3[S:17][C:16]4[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24][N:29]5[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:14][CH:15]=4)[CH2:10][C:9]=3[CH:8]=2)=[O:6])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 4875Potassium IodideHCID 8082PiperidineHCID 12340288HCID 12340288, compound

Product 1

HCID 21538544HCID 21538544, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A mixture of 40.7 g (0.10 mole) of 2,7-bis(4-chlorobutyryl)-thioxanthene, 1 g of potassium iodide and 200 ml of piperidine was stirred and heated on a steam bath for 72 hours. Upon cooling the solution was poured into 1 liter of water. The oily product obtained was dissolved in chloroform, washed with water then saturated NaCl solution, dried over magnesium sulfate and filtered. The filtrate was evaporated to a small volume, cooled, acidified to Congo Red with ethereal HCl and filtered. The resulting solid was recrystallized several times from ethanol to give the desired product. M.P. 229°-231°C.

Workup

  1. temperatureheated on a steam bath for 72 hours
  2. temperatureUpon cooling the solution
  3. customThe oily product obtained
  4. washwashed with water
  5. dry with materialsaturated NaCl solution, dried over magnesium sulfate
  6. filtrationfiltered
  7. customThe filtrate was evaporated to a small volume
  8. temperaturecooled
  9. filtrationfiltered
  10. customThe resulting solid was recrystallized several times from ethanol

Sources & evidence

ORD record
ord-117f3f4742ad493da415670509eec0c4
Source dataset
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US03957988

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes