Methyl iodide → HCID 178503863, 화합물

HRID 586561

반응식

HRID 586561 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178503863HCID 178503863, 화합물수율 74%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-a5e3c8b2da554bf685abb80ca8c18a99
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936630B2

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