Ether hydrochloride → HCID 19388477, compound

HRID 1460173Notes

Reaction equation

HRID 1460173 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[C:18]([O:21][CH3:22])[C:19]=1[OH:20])[CH2:6][N:7]1[CH2:12][CH2:11][N:10]([C:13]([S:15][CH3:16])=[S:14])[CH2:9][CH2:8]1.[ClH:23].CCOCC>C(Cl)(Cl)Cl.C[C@H]1O[C@H]2[C@H](O)[C@@H](O)[C@H](OC3C4C(=CC5OCOC=5C=4)[C@@H](C4C=C(OC)C(O)=C(OC)C=4)[C@@H]4[C@@H]3COC4=O)O[C@@H]2CO1.C1COP(NCCCl)(=O)N(CCCl)C1.[NH2-].[NH2-].Cl[Pt+2]Cl>[ClH:23].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[C:18]([O:21][CH3:22])[C:19]=1[OH:20])[CH2:6][N:7]1[CH2:8][CH2:9][N:10]([C:13]([S:15][CH3:16])=[S:14])[CH2:11][CH2:12]1

Participants

5

Reactant 2

HCID 10953452Ether hydrochlorideHCID 19388427HCID 19388427, compound

Product 1

HCID 19388477HCID 19388477, compoundYield 95.9%

Reagents, catalysts & solvents 2

HCID 56841950ICE protocol 1CatalystHCID 6212ChloroformSolvent

Procedure

In 4 ml of chloroform was dissolved 500 mg of methyl 4-(3,5-dimethoxy-4-hydroxybenzyl)-1-piperazinecarbodithioate. To the solution was dropwise added under chilling with ice 1.46 ml of 1-N HCl/ether mixture. The solvent was then distilled off under reduced pressure. The residue was stirred overnight at room temperature together with 8 ml of ethyl acetate. Precipitated crystals were collected by filtration to give 529 mg of the desired compound as a white powder, m.p. 187°-188° C. (decomp.), yield 95.9%.

Workup

  1. additionTo the solution was dropwise added
  2. distillationThe solvent was then distilled off under reduced pressure
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-f98ade111ef54de78b24733fcb5e4b2b
Source dataset
uspto-grants-1991_12
Patent number
US05070089

Reaction notes

Loading…