Lawesson's reagent → HCID 15132539, compound

HRID 2082434Notes

Reaction equation

HRID 2082434 reaction equation
[CH2:1]1[N:12]2[C:13]3[C:3](=[CH:4][CH:5]=[CH:6][C:7]=3[C:8](=O)[NH:9][C:10]3[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=32)[CH2:2]1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:28]2)=CC=1>C1(C)C=CC=CC=1>[CH2:1]1[N:12]2[C:13]3[C:3](=[CH:4][CH:5]=[CH:6][C:7]=3[C:8](=[S:28])[NH:9][C:10]3[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=32)[CH2:2]1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 15380028Dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-one

Product 1

HCID 15132539HCID 15132539, compoundYield 60.2%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To 1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-one (67 g) in 1 l of toluene, under nitrogen, was added 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (45 g). The mixture was refluxed for 1 hr and allowed to stand overnight. The precipitate was collected and recrystallized from chloroform to afford 43 g, (60.2%) of product, mp 185°-186° C.

Workup

  1. temperatureThe mixture was refluxed for 1 hr
  2. customThe precipitate was collected
  3. customrecrystallized from chloroform

Sources & evidence

ORD record
ord-084fe5f8915947d1a43a7b5e07f82989
Source dataset
uspto-grants-1993_02
Patent number
US05189161

Reaction notes

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