Butanethiol → HCID 20285387, compound

HRID 127659Notes

Reaction equation

HRID 127659 reaction equation
[CH2:1]([SH:5])[CH2:2][CH2:3][CH3:4].[H-].[Na+].Cl[CH:9]([C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=1[Cl:23])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1>O1CCCC1>[CH2:1]([S:5][CH:9]([C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=1[Cl:23])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)[CH2:2][CH2:3][CH3:4]

Participants

5

Reactant 3

HCID 8012ButanethiolHCID 24758Sodium hydrideHCID 134886161-[2-Chloro-2-(2,4-dichlorophenyl)ethyl]-1H-1,2,4-triazole

Product 1

HCID 20285387HCID 20285387, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

12.55 parts by weight of butylmercaptan is dripped into a suspension of 3.33 parts by weight of sodium hydride in 180 parts by weight of tetrahydrofuran. A solution of 27.5 parts by weight of 1-[2-chloro-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole in 50 parts of tetrahydrofuran is then dripped in and the mixture is stirred for 3 days at room temperature. The mixture is concentrated, stirred with water, and extracted with dichloromethane. The resulting dichloromethane solution is dried and evaporated. There is obtained 29.5 parts of crude 1-[2-n-butylmercapto-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole, which is dissolved in ethyl acetate. When hydrogen chloride is passed into the ethyl acetate solution, 25.9 parts of 1-[2-n-butylmercapto-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole hydrochloride, m.p. 143° C., precipitates out.

Workup

  1. concentrationThe mixture is concentrated
  2. stirringstirred with water
  3. extractionextracted with dichloromethane
  4. dry with materialThe resulting dichloromethane solution is dried
  5. customevaporated

Sources & evidence

ORD record
ord-01a85a6c040c4d478281a98218ad40d8
Source dataset
uspto-grants-1981_03
Patent number
US04256754

Reaction notes

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