Triethylamine → HCID 19020431, compound

HRID 1109597Notes

Reaction equation

HRID 1109597 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-72ae7dce69a94348974348c288db11c0
Source dataset
uspto-grants-1994_06
Patent number
US05321021

Reaction notes

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