Potassium bisulfate → HCID 54491947, compound

HRID 373038Notes

Reaction equation

HRID 373038 reaction equation
[CH2:1]([O:3][C:4]1(OCC)[CH2:9][CH2:8][C@H:7]2[C@H:10]3[C@H:19]([CH2:20][CH2:21][C@:5]12[CH3:6])[C:18]1[CH:17]=[CH:16][C:15]([O:22][CH3:23])=[CH:14][C:13]=1[CH2:12][CH2:11]3)[CH3:2].OS([O-])(=O)=O.[K+]>C1(C)C=C(C)C=C(C)C=1>[CH3:2][CH2:1][O:3][C:4]1[C@:5]2([CH2:21][CH2:20][C@H:19]3[C@@H:10]([CH2:11][CH2:12][C:13]4[CH:14]=[C:15]([O:22][CH3:23])[CH:16]=[CH:17][C:18]=43)[C@@H:7]2[CH2:8][CH:9]=1)[CH3:6]

Participants

4

Reactant 2

HCID 516920Potassium bisulfateHCID 15718549HCID 15718549, compound

Product 1

HCID 54491947HCID 54491947, compound

Reagents, catalysts & solvents 1

HCID 7947MesityleneSolvent

Procedure

5 g of 17,17-diethoxy-3-methoxy-estra-1,3,5(10)-triene is dissolved in 20 ml of mesitylene and after addition of 0.3 g of KHSO4 under inert gas is heated within 30 minutes to 40 minutes to 140° C. to 160° C. and is gradually distilled off from the solvent. Then, it is heated for 2 more hours in a vacuum at this temperature and the remaining solvent is distilled off. The remaining residue is used in the next step in the form of an oil without purification. IR[cm-1 ]: 1500, 1575, 1620 (aromatic); 1620 (enol ether superimposed).

Workup

  1. temperatureis heated within 30 minutes to 40 minutes to 140° C. to 160° C.
  2. distillationis gradually distilled off from the solvent
  3. temperatureThen, it is heated for 2 more hours in a vacuum at this temperature
  4. distillationthe remaining solvent is distilled off
  5. customThe remaining residue is used in the next step in the form of an oil without purification

Sources & evidence

ORD record
ord-c822a9c33b7244619f14a354c9d568bf
Source dataset
uspto-grants-1992_11
Patent number
US05162312

Reaction notes

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