Triethylamine → HCID 13823416, compound

HRID 1906371Notes

Reaction equation

HRID 1906371 reaction equation
[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[C:6]1[SH:16])[CH2:2][CH2:3][CH3:4].Cl[Sn:18]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(N(CC)CC)C>C(Cl)Cl>[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[C:6]1[S:16][Sn:18]([C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[CH2:2][CH2:3][CH3:4]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 12540Triphenyltin ChlorideHCID 178448728HCID 178448728, compound2×

Product 1

HCID 13823416HCID 13823416, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 0.85 g (0.004 mole) 3-n-butyl-2-mercapto-4(3H)-quinazolinone (the product of Example 6), 1.54 g (0.004 mole) chlorotriphenyl tin and 0.4 g (0.004 mole) triethylamine in methylene chloride (about 100 ml) was stirred for one hour, refluxed 5.5 hours, stirred overnight and refluxed 8 hours. The reaction mixture was washed with water. The organic phase was dried over magnesium sulfate, and stripped to obtain the above-identified product as a solid, melting point 112° to 114° C.

Workup

  1. temperaturerefluxed 5.5 hours
  2. stirringstirred overnight
  3. temperaturerefluxed 8 hours
  4. washThe reaction mixture was washed with water
  5. dry with materialThe organic phase was dried over magnesium sulfate

Sources & evidence

ORD record
ord-d4b155d8c40843af9bfd07ff3e9e55d4
Source dataset
uspto-grants-1987_03
Patent number
US04652558

Reaction notes

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