Methyl iodide → HCID 178503863、化合物

HRID 1282219

反応式

HRID 1282219 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:20])=[C:6]([NH:8][C:9]([NH:11][C:12]2[C:13]([CH3:19])=[N:14][N:15]([CH3:18])[C:16]=2[CH3:17])=[S:10])[CH:7]=1.[CH3:21]I>CC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:20])=[C:6]([NH:8]/[C:9](=[N:11]\[C:12]2[C:13]([CH3:19])=[N:14][N:15]([CH3:18])[C:16]=2[CH3:17])/[S:10][CH3:21])[CH:7]=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 98578071-(5-Chloro-2-methyl-phenyl)-3-(1,3,5-trimethyl-1H-pyrazol-4-yl)-thiourea

生成物 1

HCID 178503863HCID 178503863、化合物収率 74%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Under anhydrous conditions, a solution of 1-(5-Chloro-2-methyl-phenyl)-3-(1,3,5-trimethyl-1H-pyrazol-4-yl)-thiourea (2.3 g, 7.5 mmol) produced in example 8 and methyl iodide (0.94 mL, 15 mmol) in 70 mL of acetone was stirred at ambient temperature for 64 hours. The reaction mixture was concentrated in vacuo and partitioned between CH2Cl2 and saturated aqueous NaHCO3 solution. The organic phase was washed with dilute Na2S2O3 and dried (Na2SO4). Removal of solvent and crystallization of the residue from Et2O provided 1.78 g of title compound as a white solid (74% of theory, m.p. 134-135° C.).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. custompartitioned between CH2Cl2 and saturated aqueous NaHCO3 solution
  3. washThe organic phase was washed with dilute Na2S2O3
  4. dry with materialdried (Na2SO4)
  5. customRemoval of solvent and crystallization of the residue from Et2O

出典と根拠

ORDレコード
ord-5f9535551aba4e93b618843363ab3f51
出典データセット
uspto-grants-2002_09
特許番号
US06455566B1

関連ノート

読み込み中…