Acetic Acid → HCID 178517892, compound

HRID 70094

Reaction equation

HRID 70094 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(O)(=O)C.CS[C:20]1[N:21]=[C:22]([OH:29])[C:23]2[S:28][CH2:27][CH2:26][C:24]=2[N:25]=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:20]3[N:21]=[C:22]([OH:29])[C:23]4[S:28][CH2:27][CH2:26][C:24]=4[N:25]=3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 974781-(4-Chlorophenyl)piperazineHCID 178503521HCID 178503521, compound

Product 1

HCID 178517892HCID 178517892, compoundYield 92.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
180 °C

Procedure

20.45 g 1-(4-chloro-phenyl)-piperazine are placed in 5.95 ml (104 mmol) glacial acetic acid and heated to 180° C. 8.01 g 2-methylsulphanyl-6,7-dihydro-thieno[3,2-d]pyrimidin-4-ol are added, the non-stirrable reaction mixture is heated for 2.5 hours to 180° C. After cooling, water is added, the precipitate is suction filtered and dried in the air. The substance is treated with ethanol under ultrasound, suction filtered and dried. 12.95 g of the product are obtained as a powder.

Workup

  1. temperaturethe non-stirrable reaction mixture is heated for 2.5 hours to 180° C
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. customdried in the air
  5. additionThe substance is treated with ethanol under ultrasound, suction
  6. filtrationfiltered
  7. customdried

Sources & evidence

ORD record
ord-115cf9f5eb3a4b0b9a4d930d5c814dda
Source dataset
uspto-grants-2014_09
Patent number
US08822474B2

Linked notes

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