Lawesson's reagent → HCID 86629622, compound

HRID 911380Notes

Reaction equation

HRID 911380 reaction equation
[C:1]([NH:5][C:6]([C:8]1[CH:27]=[CH:26][C:11]([CH2:12][NH:13][C:14]2[C:24]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19][C:18]=3[CH:17]=[CH:16][C:15]=2[Cl:25])=[CH:10][CH:9]=1)=O)([CH3:4])([CH3:3])[CH3:2].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:37]2)=CC=1>O1CCOCC1>[ClH:25].[Cl:25][C:15]1[CH:16]=[CH:17][C:18]2[CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]=2[C:14]=1[NH:13][CH2:12][C:11]1[CH:26]=[CH:27][C:8]([C:6](=[S:37])[NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:9][CH:10]=1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 57655999HCID 57655999, compound

Product 1

HCID 86629622HCID 86629622, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Combine 6-(4-tert-butylcarbamoyl-benzylamino)-7-chloro-2,3,4,5-tetrahydro-1H-benzo-[d]azepine (0.3 g, 0.67 mmol), 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's reagent) (0.3, g, 0.67 mmol) and anhydrous 1,4-dioxane (10 mL) in a sealed tube and heat at 100° C. for 5 h. Cool the reaction mixture to ambient temperature, evaporate the solvent and purify the residue by SCX

Workup

  1. customevaporate the solvent
  2. custompurify the residue by SCX

Sources & evidence

ORD record
ord-d5f5417a52ea4b1885cb25c78da56812
Source dataset
uspto-grants-2011_09
Patent number
US08022062B2

Reaction notes

Loading…