Thiomorpholine → HCID 54591023, compound

HRID 1619976Notes

Reaction equation

HRID 1619976 reaction equation
[CH3:1][CH:2]1[C:7]([C:8]2[CH:18]=[CH:17][C:11]3[N:12]=[C:13](SC)[O:14][C:10]=3[CH:9]=2)=[N:6][NH:5][C:4](=[O:19])[CH2:3]1.[NH:20]1[CH2:25][CH2:24][S:23][CH2:22][CH2:21]1>>[CH3:1][CH:2]1[C:7]([C:8]2[CH:18]=[CH:17][C:11]3[N:12]=[C:13]([N:20]4[CH2:25][CH2:24][S:23][CH2:22][CH2:21]4)[O:14][C:10]=3[CH:9]=2)=[N:6][NH:5][C:4](=[O:19])[CH2:3]1

Participants

3

Reactant 2

HCID 67164ThiomorpholineHCID 17993492HCID 17993492, compound

Product 1

HCID 54591023HCID 54591023, compound

Conditions

Temperature
130 °C

Procedure

A mixture of 4.1 g (0.015 mol) 5-methyl-6-(2-methylsulphanyl-benzoxazol-6-yl)-4,5-dihydro-2H-pyridazin-3-one and 10.3 g (0.1 mol) thiomorpholine is stirred for 6 h at 130° C. Then the excess thiomorpholine is eliminated by rotary evaporation in vacuo, the residue is stirred with water and diisopropylether, the crystals obtained are suction filtered. The crude product is washed with water and isopropanol and then recrystallised from aqueous isopropanol.

Workup

  1. customThen the excess thiomorpholine is eliminated by rotary evaporation in vacuo
  2. stirringthe residue is stirred with water and diisopropylether
  3. customthe crystals obtained
  4. washThe crude product is washed with water and isopropanol
  5. customrecrystallised from aqueous isopropanol

Sources & evidence

ORD record
ord-f154514066c74e8499a067c2db3d468a
Source dataset
uspto-grants-2014_07
Patent number
US08772323B2

Reaction notes

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