Water → HCID 14547402, compound

HRID 543130Notes

Reaction equation

HRID 543130 reaction equation
[CH:1]1([C:7]([S:9]C)=S)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:11]=[C:12]1[N:17]2[CH2:18][CH2:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[CH:16]2[CH2:15][NH:14][CH2:13]1.O>CN(C)C=O>[CH:1]1([C:7]([N:14]2[CH2:13][C:12](=[O:11])[N:17]3[CH2:18][CH2:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH:16]3[CH2:15]2)=[S:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

5

Reactant 3

HCID 962WaterHCID 11401064HCID 11401064, compoundHCID 14547364HCID 14547364, compound

Product 1

HCID 14547402HCID 14547402, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

Methyl cyclohexanecarbodithioate (0.24 g) was added to a solution of 4-oxo-1,2,3,4,6,7,8,12b-octahydropyrazino[2,1-a][2]benzazepine (0.3 g) in dimethylformamide (5 ml). The mixture was refluxed for 4 h, cooled and poured into water. This was extracted with diethyl ether; the ether solution was dried (MgSO4) and evaporated. The residue was purified by column chromatography (SiO2, diethyl ether).

Workup

  1. temperatureThe mixture was refluxed for 4 h
  2. temperaturecooled
  3. extractionThis was extracted with diethyl ether
  4. dry with materialthe ether solution was dried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by column chromatography (SiO2, diethyl ether)

Sources & evidence

ORD record
ord-99f4d0c9f4994c13bf56839caf414f7c
Source dataset
uspto-grants-1987_04
Patent number
US04661489

Reaction notes

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