Lawesson's reagent → HCID 178432332, compound
Reaction equation
[CH3:1][N:2]1[CH:7]=[C:6]([CH:8]2[C:14]3[N:15]=[C:16]([CH3:18])[NH:17][C:13]=3[CH:12]=[CH:11][C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]2=3)[C:5](=O)[NH:4][C:3]1=[O:24].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:34])=CC=1>>[CH3:1][N:2]1[CH:7]=[C:6]([CH:8]2[C:14]3[N:15]=[C:16]([CH3:18])[NH:17][C:13]=3[CH:12]=[CH:11][C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]2=3)[C:5](=[S:34])[NH:4][C:3]1=[O:24]Participants
3
Procedure
The title product was prepared from the product of step (iv) (0.1 g) and Lawesson's reagent (0.378 g) according to the method of example 34 step (iv). Purification was by chromatography eluting with 0-5% methanol in dichloromethane followed by reverse phase HPLC using a 40 mm Novapak column eluting with 15-85% methanol in 0.1% aqueous ammonium acetate gradient over 9 min.
Workup
- customPurification
- washeluting with 0-5% methanol in dichloromethane
- washeluting with 15-85% methanol in 0.1% aqueous ammonium acetate gradient over 9 min.
Sources & evidence
- ORD record
- ord-3ae2a5d1a6034d569fe816fd86565124
- Source dataset
- uspto-grants-2001_04
- Patent number
- US06218376B1
Reaction notes
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