Hydrochloric Acid → HCID 12374929, compound

HRID 1732776Notes

Reaction equation

HRID 1732776 reaction equation
[Cl-:1].[Ca+2].[Cl-].[Cl:4][C:5]1[C:6]([F:22])=[CH:7][C:8]2[S:14][C:13]3[CH:15]=[C:16]([F:19])[CH:17]=[CH:18][C:12]=3[CH2:11][CH:10](O)[C:9]=2[CH:21]=1.Cl>C(Cl)Cl>[Cl:4][C:5]1[C:6]([F:22])=[CH:7][C:8]2[S:14][C:13]3[CH:15]=[C:16]([F:19])[CH:17]=[CH:18][C:12]=3[CH2:11][CH:10]([Cl:1])[C:9]=2[CH:21]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 12374925HCID 12374925, compound

Product 1

HCID 12374929HCID 12374929, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Powdered anhydrous calcium chloride (5 g) was added to a solution of the alcohol from the preceding preparation (7.6 g) in methylene chloride (100 ml) and anhydrous hydrogen chloride introduced into the suspension for 2 hours. The mixture was then allowed to stand overnight and filtered. The filtrate was evaporated, yielding 7.5 g of the desired 8,10-dichloro-3,7-difluoro-10,11-dihydrodibenzo(b,f)thiepine which is crystallized from cyclohexane. The pure compound melts at 118.5°-119.5° C.

Workup

  1. filtrationfiltered
  2. customThe filtrate was evaporated

Sources & evidence

ORD record
ord-2263be9fb3da4fcf87c2de72a08e99a2
Source dataset
uspto-grants-1980_12
Patent number
US04238611

Reaction notes

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