1,5-Diazabicyclo(4.3.0)non-5-ene → HCID 12881671, compound
Reaction equation
[CH3:1][N:2]1[C:6](=[S:7])[N:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[C:4](=[O:15])[N:3]1[CH2:16][CH2:17]Br.N12CCCC1=NCCC2>C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:6](=[S:7])[N:5]([C:8]2[CH:9]=[CH:10][C:11]([Cl:14])=[CH:12][CH:13]=2)[C:4](=[O:15])[N:3]1[CH:16]=[CH2:17]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 5.9 g of 1-methyl-2-(2-bromoethyl)-4-(4-chlorophenyl)-1,2,4-triazolidin-3-one-5-thione (prepared as in Example 3) and 2.1 g 1,5-diaza-bicyclo[4.3.0] non-5-ene in 100 ml chloroform was heated to reflux for 3 hours and stirred overnight at room temperature. The mixture was washed with water, dried (MgSO4), stripped and chromatographed by high-pressure liquid chromatography. Yield: 2.6 g.
Workup
- temperaturewas heated
- temperatureto reflux for 3 hours
- washThe mixture was washed with water
- dry with materialdried (MgSO4)
- customchromatographed by high-pressure liquid chromatography
Sources & evidence
- ORD record
- ord-99735297aedd4665921ffb6385185200
- Source dataset
- uspto-grants-1982_04
- Patent number
- US04326878
Reaction notes
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