Lawesson's reagent → HCID 23366702, compound

HRID 1079340Notes

Reaction equation

HRID 1079340 reaction equation
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=O)[CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:22])=CC=1>C1(C)C=CC=CC=1>[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=[S:22])[CH2:2]1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 41786501,4-Benzothiazepin-3(2H)-one, 4,5-dihydro-

Product 1

HCID 23366702HCID 23366702, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
100 °C

Procedure

A stirred mixture of 4,5-dihydro-1,4-benzothiazepin-3(2H)-one (1.79 g, prepared as example 1 of international patent application WO 92/21668) and Lawesson's reagent (2.22 g) in dry toluene (100 ml) was heated at 100° C. for three hours. The mixture was allowed to cool to room temperature. The precipitated solid was collected by filtration, washed with toluene and dried to give 4,5-dihydro-1,4-benzothiazepin-3(2H)-thione. Yield 1.78 g (m.p. 215°-219° C.).

Workup

  1. temperatureto cool to room temperature
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with toluene
  4. customdried

Sources & evidence

ORD record
ord-7310f321071e48f4845a14ce9814a9d4
Source dataset
uspto-grants-1996_12
Patent number
US05580866

Reaction notes

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