Benzene → HCID 12271978, compound

HRID 1732758Notes

Reaction equation

HRID 1732758 reaction equation
[Cl:1][C:2]1[C:27]([Cl:28])=[CH:26][C:5]2[CH:6]([N:15]3[CH2:20][CH2:19][N:18](C(OCC)=O)[CH2:17][CH2:16]3)[CH2:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=3[S:10][C:4]=2[CH:3]=1.[OH-].[K+].C(O)C.C1C=CC=CC=1>O>[Cl:1][C:2]1[C:27]([Cl:28])=[CH:26][C:5]2[CH:6]([N:15]3[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]3)[CH2:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=3[S:10][C:4]=2[CH:3]=1

Participants

6

Reactant 4

HCID 241BenzeneHCID 702EthanolHCID 14797Potassium HydroxideHCID 12271976HCID 12271976, compound

Product 1

HCID 12271978HCID 12271978, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The same product was prepared by the following procedure: A mixture of crude 7,8-dichloro-10-(4-ethoxycarbonylpiperazino)-10,11-dihydrodibenzo(b,f)thiepine (3.5 g) (prepared according to the preceding Example), potassium hydroxide (1.75 g) and ethanol (3.5 ml) was refluxed for 3 hours in a bath heated to 120°-125° C. The reaction mixture was cooled and shaken with benzene and water. The isolation procedure is the same as described in the preceding Examples, yielding the crude base in an almost theoretical yield. On crystallization from acetone it melts at 131°-133° C.

Workup

  1. customThe same product was prepared by the following procedure
  2. customprepared
  3. temperaturewas refluxed for 3 hours in a bath
  4. temperatureheated to 120°-125° C
  5. temperatureThe reaction mixture was cooled

Sources & evidence

ORD record
ord-041f70a0ee574d4594cbd6ab399bebec
Source dataset
uspto-grants-1980_12
Patent number
US04238611

Reaction notes

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