Acetic Acid → 8-Aminodibenzo[b,f]thiepin-3-carboxylic Acid Hydrochloride Salt

HRID 485441Notes

Reaction equation

HRID 485441 reaction equation
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=C(C#N)[CH:14]=[CH:15][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:18]=1.[ClH:19].[C:20]([OH:23])(=[O:22])[CH3:21]>>[ClH:19].[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[C:21]([C:20]([OH:23])=[O:22])[CH:14]=[CH:15][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:18]=1

Participants

4

Reactant 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 131518838-Amino-3-cyanodibenzo[b,f]thiepin

Product 1

HCID 131518868-Aminodibenzo[b,f]thiepin-3-carboxylic Acid Hydrochloride Salt

Procedure

850 Mg. 8-amino-3-cyanodibenzo[b,f]thiepin is refluxed in a mixture of 20 cc. acetic acid and 20 cc. concentrated hydrochloric acid for 48 hours. The suspended solid is filtered, washed with some acetic acid, dried overnight under vacuum at 70° C. to yield 600 mg. pure compound, m.p. 308°-311° C.

Workup

  1. filtrationThe suspended solid is filtered
  2. washwashed with some acetic acid
  3. customdried overnight under vacuum at 70° C.
  4. customto yield 600 mg

Sources & evidence

ORD record
ord-0c386a8e0a534979a630886e6d209f2f
Source dataset
uspto-grants-1985_08
Patent number
US04536507

Reaction notes

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