Potassium Carbonate → HCID 57425811, 화합물

HRID 1363641노트

반응식

HRID 1363641 반응식
[CH3:1][C:2]1[S:6][C:5]([CH2:7]CS([O-])(=O)=O)=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].FC(F)(F)C1N=C(C(F)(F)F)NN=1.C(=O)([O-])[O-:30].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C>[CH3:1][C:2]1[S:6][C:5]([CH2:7][OH:30])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 146885163,5-Bis(trifluoromethyl)-1H-1,2,4-triazoleHCID 86626337HCID 86626337, 화합물

생성물 1

HCID 57425811HCID 57425811, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1.0 g (3.98 mmol) (5-methyl-4-nitro-2-thienyl)methylmethane sulphonate, 0.82 g (3.98 mmol) 3,5-bis(trifluoromethyl)-1H-1,2,4-triazole, 0.93 g (5.97 mmol) potassium carbonate and 0.11 g (0.398 mmol) 18-crown-6 are heated under reflux in acetonitrile for 2 h. The cooled reaction mixture is evaporated, the residue taken up in 20 ml water and extracted three times with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution, dried over sodium sulphate and the solvent is distilled off under vacuum. The product (1-[(5-methyl-4-nitro-2-thienyl)methyl]-3,5-bis(trifluoromethyl)-1H-1,2,4-triazole) is used in the next stage without purification.

후처리

  1. customThe cooled reaction mixture
  2. customis evaporated
  3. extractionextracted three times with ethyl acetate
  4. washThe combined organic phases are washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulphate
  6. distillationthe solvent is distilled off under vacuum
  7. customThe product (1-[(5-methyl-4-nitro-2-thienyl)methyl]-3,5-bis(trifluoromethyl)-1H-1,2,4-triazole) is used in the next stage without purification

출처 및 근거

ORD 기록
ord-cfca1f7d771c48d9bd45b50a59b49e03
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07884242B2

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