聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → [5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide

HRID 25279

反应方程式

HRID 25279 反应方程式
[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]

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 63622-碘代丙烷HCID 221709441,1'-Thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene]HCID 23689980次硫酸氢钠甲醛

产物 1

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

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

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 dtied 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).

后处理

  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. distillationthe ethyl acetate was distilled off under reduced pressure
  5. customPurification of the residue by silica gel column chromatography

来源与证据

ORD记录
ord-6874889d9b6847a0840fc9cf974c3a49
来源数据集
uspto-grants-2005_02
专利号
US06858639B2

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