2-Thiophenethiol → HCID 23462914, compound

HRID 2286392Notes

Reaction equation

HRID 2286392 reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[SH:6].[CH3:7][N:8]1[CH2:14][CH2:13][C:12]2=[CH:15][C:16](=[O:20])[C:17](=[O:19])[CH:18]=[C:11]2[CH2:10][CH2:9]1>CO>[OH:20][C:16]1[C:17]([OH:19])=[CH:18][C:11]2[CH2:10][CH2:9][N:8]([CH3:7])[CH2:14][CH2:13][C:12]=2[C:15]=1[S:6][C:2]1[S:1][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 5226742-ThiophenethiolHCID 12668030HCID 12668030, compound

Product 1

HCID 23462914HCID 23462914, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred solution of 2-thiophenethiol (0.9 g., 0.0076 mole) in 200 ml. of methanol was added portionwise 2 g. (0.0074 mole) of 3-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7,8-dione, at room temperature under argon. After stirring for 1 hour, the methanol was distilled under vacuum, the residue slurried in 30 ml. of water and filtered. The filtrate was made basic to give the product, 7,8-dihydroxy-3-methyl-6-(2-thienylthio)-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 189°-191° C.

Workup

  1. customat room temperature
  2. distillationthe methanol was distilled under vacuum
  3. filtrationof water and filtered

Sources & evidence

ORD record
ord-820dcb54baae4c669c5acada03973643
Source dataset
uspto-grants-1981_05
Patent number
US04265890

Reaction notes

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