HCID 73792980, compound → HCID 21469779, compound

HRID 1938640Notes

Reaction equation

HRID 1938640 reaction equation
Cl.[CH2:2]([N:4]([CH2:31][CH3:32])[CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[Cl:18])=[CH:12][CH:11]=1)[CH3:3]>O1CCCC1>[ClH:18].[CH2:31]([N:4]([CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13](/[C:16](/[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:17](\[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)/[Cl:18])=[CH:12][CH:11]=1)[CH3:32]

Participants

3

Reactant 1

HCID 73792980HCID 73792980, compound

Product 1

HCID 21469779HCID 21469779, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
30 °C

Procedure

Combine (E and Z)-1-[4-(4-diethylaminobutoxy)phenyl]-1,2-diphenyl-2-chloro-ethylene hydrochloride salt (21.5 mol) and tetrahydrofuran (75 L). Heat to reflux. After 1 hour, cool to 30° C. to give a solid. Collect the solid by filtration, rinse with tetrahydrofuran, and dry. Combine the solid with tetrahydrofuran (83.2 L) and heat to reflux. After 18 hour, cool to 50° C. and filter, rinse with tetrahydrofuran, and dry to give (E)-1-[4-(4-diethylaminobutoxy)phenyl]-1,2-diphenyl-2-chloro-ethylene hydrochloride salt.

Workup

  1. temperatureHeat to reflux
  2. customto give a solid
  3. customCollect the solid
  4. filtrationby filtration
  5. washrinse with tetrahydrofuran
  6. customdry
  7. temperatureheat to reflux
  8. waitAfter 18 hour
  9. temperaturecool to 50° C.
  10. filtrationfilter
  11. washrinse with tetrahydrofuran
  12. customdry

Sources & evidence

ORD record
ord-1c5cb495399e4192823bb2b2d6966b9a
Source dataset
uspto-grants-1997_12
Patent number
US05693674

Reaction notes

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