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

HRID 1635719

반응식

HRID 1635719 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>[Cl:19][C:9]1[CH:10]=[C:11]([C:15]([F:17])([F:18])[F:16])[CH:12]=[C:13]([Cl:14])[C:8]=1[C:6]1[CH:5]=[CH:4][C:3]([CH3:20])=[C:2]([S:1][CH:21]([CH3:22])[CH3:26])[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6362Isopropyl iodideHCID 221709441,1'-Thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene]HCID 23689980Sodium Formaldehyde Sulfoxylate

생성물 1

HCID 12137642[5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide수율 75.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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-aa532dc4379e45f38b0b5e730b621edb
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509354B1

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