Hydrochloric Acid → HCID 12374931, compound

HRID 1732779Notes

Reaction equation

HRID 1732779 reaction equation
[ClH:1].[Cl:2][C:3]1[C:4]([O:21][CH3:22])=[CH:5][C:6]2[S:12][C:11]3[CH:13]=[C:14]([O:17][CH3:18])[CH:15]=[CH:16][C:10]=3[CH2:9][CH:8](O)[C:7]=2[CH:20]=1.[Cl-].[Ca+2].[Cl-]>C(Cl)Cl>[Cl:2][C:3]1[C:4]([O:21][CH3:22])=[CH:5][C:6]2[S:12][C:11]3[CH:13]=[C:14]([O:17][CH3:18])[CH:15]=[CH:16][C:10]=3[CH2:9][CH:8]([Cl:1])[C:7]=2[CH:20]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 12374927HCID 12374927, compound

Product 1

HCID 12374931HCID 12374931, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Anhydrous hydrogen chloride was passed at 0° C. into a stirred solution of the alcohol from the above experiment (22.5 g) in methylene chloride (500 ml) for 3 hours. Anhydrous calcium chloride (5 g) was added, the mixture stirred at room temperature for 3 hours and filtered. The filtrate was evaporated under diminished pressure, yielding 23.4 g of crude 8,10-dichloro-3,7-dimethoxy-10,11-dihydrodibenzo(b,f)-thiepine. The compound was crystallized from methylene chloride and melted in the pure state at 151°-153° C.

Workup

  1. filtrationfiltered
  2. customThe filtrate was evaporated under diminished pressure

Sources & evidence

ORD record
ord-0f1f94fc22c2488fb10fbde1318d9776
Source dataset
uspto-grants-1980_12
Patent number
US04238611

Reaction notes

Loading…