碳酸钾 → (2-Ethoxymethoxy-5-(4-trifluoromethylphenyl)phenyl] 2,2,2-trifluoroethyl sulfide

HRID 25280

反应方程式

HRID 25280 反应方程式
[S:1]([C:23]1[CH:28]=[C:27]([C:29]2[CH:34]=[CH:33][C:32]([C:35]([F:38])([F:37])[F:36])=[CH:31][CH:30]=2)[CH:26]=[CH:25][C:24]=1[O:39][CH2:40][O:41][CH2:42][CH3:43])C1C=C(C2C=CC(C(F)(F)F)=CC=2)C=CC=1OCOCC.C(S([O-])=O)O.[Na+].C(=O)([O-])[O-].[K+].[K+].[F:56][C:57]([F:61])([F:60])[CH2:58]I>CN(C)C=O.O>[F:56][C:57]([F:61])([F:60])[CH2:58][S:1][C:23]1[CH:28]=[C:27]([C:29]2[CH:34]=[CH:33][C:32]([C:35]([F:37])([F:36])[F:38])=[CH:31][CH:30]=2)[CH:26]=[CH:25][C:24]=1[O:39][CH2:40][O:41][CH2:42][CH3:43]

参与物

7

反应物 4

HCID 11430碳酸钾HCID 677092-碘-1,1,1-三氟乙烷HCID 221708901,1'-Thiodi-[2-ethoxymethoxy-5-(4-trifluoromethylphenyl)benzene]HCID 23689980次硫酸氢钠甲醛

产物 1

HCID 86587598(2-Ethoxymethoxy-5-(4-trifluoromethylphenyl)phenyl] 2,2,2-trifluoroethyl sulfide收率 151.1%

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

3.3 g (5.0 mmol) of 1,1′-thiodi-[2-ethoxymethoxy-5-(4-trifluoromethylphenyl)benzene], 3.0 g (19.5 mmol) of Rongalite, 3.0 g (21.7 mmol) of potassium carbonate and 3.2 g (17.6 mmol) of 2,2,2-trifluoroethyl iodide were stirred in 50 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 3.1 g of (2-ethoxymethoxy-5-(4-trifluoromethylphenyl)phenyl] 2,2,2-trifluoroethyl sulfide (yield 75.6%) as a pale yellow viscous liquid (nD20 1.5213).

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. 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

来源与证据

ORD记录
ord-c3157614ddee40f7b889ddcb92241301
来源数据集
uspto-grants-2005_02
专利号
US06858639B2

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