Diethyl Ether → HCID 20034081, compound

HRID 231645Notes

Reaction equation

HRID 231645 reaction equation
[C:1]([CH:3]1[CH2:7][S:6][CH2:5][C:4]1=O)#[N:2].[ClH:9].[NH2:10]O.CCOCC>C(#N)C>[ClH:9].[NH2:10][C:4]1[C:3]([C:1]#[N:2])=[CH:7][S:6][CH:5]=1

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 3266764-Cyano-3-tetrahydrothiophenoneHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 20034081HCID 20034081, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

4-Cyano-3-oxotetrahydrothiophene (1.27 g) was dissolved in acetonitrile (15 ml) with heating and stirring. Hydroxylamine hydrochloride (0.69 g) was added to the refluxing solution and the mixture was refluxed for 11/2hour. After cooling, ether (25 ml) was added and the title compound was filtered off and air-dried. Yield 1.35 g (84%); mp 244°-246°. δ'H nmr (CDCl3 /DMSO-d6) 9.2(br s) 8.55 (d, J=4Hz) 7.85 (d, J=4Hz).

Workup

  1. temperaturewith heating
  2. temperaturethe mixture was refluxed for 11/2hour
  3. temperatureAfter cooling
  4. filtrationthe title compound was filtered off
  5. customair-dried

Sources & evidence

ORD record
ord-e27f678ce22145ba924dd6613a18fb38
Source dataset
uspto-grants-1989_07
Patent number
US04847386

Reaction notes

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