Water → [5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide

HRID 1432737

반응식

HRID 1432737 반응식
[S:1]([C:21]1[CH:26]=C(C2C(Cl)=CC(C(F)(F)F)=CC=2Cl)C=C[C:22]=1C)[C:2]1[CH:7]=[C:6]([C:8]2[C:13]([Cl:14])=[CH:12][C:11]([C:15]([F:18])([F:17])[F:16])=[CH:10][C:9]=2[Cl:19])[CH:5]=[CH:4][C:3]=1[CH3:20].C(S([O-])=O)O.[Na+].C(I)(C)C.O>CN(C)C=O>[CH:21]([S:1][C:2]1[CH:7]=[C:6]([C:8]2[C:9]([Cl:19])=[CH:10][C:11]([C:15]([F:18])([F:16])[F:17])=[CH:12][C:13]=2[Cl:14])[CH:5]=[CH:4][C:3]=1[CH3:20])([CH3:26])[CH3:22]

참가 물질

6

실험 절차

3.3 g (4.9 mmol) of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene], 3.0 g (19.5 mmol) of Rongalite and 3.0 g (17.6 mmol) of isopropyl iodide were stirred in 30 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.4 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl] isopropyl sulfide (yield 38.0%) as a yellow dough (nD20 1.5462).

후처리

  1. customThe resulting reaction mixture
  2. extractionextracted with 50 ml of ethyl acetate twice
  3. washThe ethyl acetate layer was washed with 50 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe ethyl acetate was distilled off under reduced pressure
  6. customPurification of the residue by silica gel column chromatography

출처 및 근거

ORD 기록
ord-b82084e543554e1babc247c99d74598d
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612105B2

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