Triethylamine → HCID 19020431, compound

HRID 477950Notes

Reaction equation

HRID 477950 reaction equation
[S:1]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[C:5](=[S:11])[NH:4][CH2:3][CH2:2]1.S(NN=[C:24]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:25](Cl)=[O:26])(C1C=CC(C)=CC=1)(=O)=[O:13].C(N(CC)CC)C>C(Cl)Cl>[OH-:13].[OH:26][C:25]1[N+:4]2[CH2:3][CH2:2][S:1][C:7]3[CH:8]=[CH:9][S:10][C:6]=3[C:5]=2[S:11][C:24]=1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 11446993HCID 11446993, compoundHCID 57310872HCID 57310872, compound

Product 1

HCID 19020431HCID 19020431, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

0.6 g of 3,4-dihydro-thieno[2,3-f][1,4]thiazepine-5(2H)-thione and 1.0 g of α-(tosylhydrazono)phenylacetyl chloride were stirred for a long time in 50 ml of methylene chloride at room temperature and in the presence of 0.84 ml of triethylamine. The solvent was removed in vacuo and the residue was chromatographed on silica gel. There was obtained 5,6-dihydro-8-hydroxy-9-phenyl-thiazolo[3,2-d]thieno[2,3-f][1,4]thiazepinium hydroxide (internal salt) of m.p. 190°-195°.

Workup

  1. customThe solvent was removed in vacuo
  2. customthe residue was chromatographed on silica gel

Sources & evidence

ORD record
ord-0f91756a56b340f69678936ea41d996f
Source dataset
uspto-grants-1989_12
Patent number
US04889848

Reaction notes

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