Hydrochloric Acid → HCID 12232366, compound

HRID 435704Notes

Reaction equation

HRID 435704 reaction equation
[F:1][C:2]1[CH:17]=[CH:16][C:5]2[S:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9](O)[CH2:10][C:4]=2[CH:3]=1.[Cl-:18].[Ca+2].[Cl-].Cl>C1C=CC=CC=1>[Cl:18][CH:9]1[C:8]2[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=2[S:6][C:5]2[CH:16]=[CH:17][C:2]([F:1])=[CH:3][C:4]=2[CH2:10]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 12232362HCID 12232362, compound

Product 1

HCID 12232366HCID 12232366, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

21.2 g of 2-fluoro-10,11-dihydro-dibenzo[b,f]thiepin-10-ol, 110 ml of benzene and 7.9 g of finely powdered calcium chloride are saturated with hydrochloric acid gas at 15° C (2 hours). The precipitate is filtered off and washed with benzene. The filtrate is evaporated under reduced pressure. There is obtained 10-chloro-2-fluoro-10,11-dihydro-dibenzo[b,f]thiepin as pink crystals which melt at 90°-92° C.

Workup

  1. custom(2 hours)
  2. filtrationThe precipitate is filtered off
  3. washwashed with benzene
  4. customThe filtrate is evaporated under reduced pressure

Sources & evidence

ORD record
ord-316a1d534daa42c2b29c4f0ee2139cbe
Source dataset
uspto-grants-1977_02
Patent number
US04006144

Reaction notes

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