Hydrochloric Acid → HCID 13050677, compound

HRID 1389282Notes

Reaction equation

HRID 1389282 reaction equation
[Cl-:1].[Ca+2].[Cl-].[CH2:4]([C:6]1[CH:7]=[CH:8][C:9]2[S:15][C:14]3[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:13]=3[CH2:12][CH:11](O)[C:10]=2[CH:22]=1)[CH3:5].Cl>C1C=CC=CC=1>[Cl:1][CH:11]1[C:10]2[CH:22]=[C:6]([CH2:4][CH3:5])[CH:7]=[CH:8][C:9]=2[S:15][C:14]2[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:13]=2[CH2:12]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 15581165HCID 15581165, compound

Product 1

HCID 13050677HCID 13050677, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

Powdered anhydrous calcium chloride (9 g) was added to a solution of 9.4 g of the foregoing alcohol in 120 ml of benzene and the suspension saturated over 2 hours under stirring with anhydrous hydrogen chloride. After 1 hour standing, the mixture was filtered, and the filtrate evaporated under reduced pressure. The required 10-chloro-8-ethyl-3-fluoro-10,11-dihydrodibenzo(b,f)thiepin was obtained in an almost theoretical yield (10.0 g); crystallization from petroleum ether yielded the pure substance melting at 68°-70° C.

Workup

  1. filtrationthe mixture was filtered
  2. customthe filtrate evaporated under reduced pressure

Sources & evidence

ORD record
ord-0dd8ff59f2d74e82a75d294177f332a0
Source dataset
uspto-grants-1981_01
Patent number
US04243805

Reaction notes

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