Potassium Carbonate → HCID 57425811、化合物

HRID 1363641ノート

反応式

HRID 1363641 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 57425811HCID 57425811、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cfca1f7d771c48d9bd45b50a59b49e03
出典データセット
uspto-grants-2011_02
特許番号
US07884242B2

反応ノート

読み込み中…