Sodium Iodide → HCID 54270636、化合物

HRID 55364

反応式

HRID 55364 の反応式
Cl[Si:2]([CH3:5])([CH3:4])[CH3:3].C(N(CC)CC)C.[CH3:13][CH2:14][C:15]([C:17]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=1)=[O:16].[I-].[Na+]>C(#N)C>[Cl:23][C:20]1[CH:19]=[CH:18][C:17]([C:15]([O:16][Si:2]([CH3:5])([CH3:4])[CH3:3])=[CH:14][CH3:13])=[CH:22][CH:21]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 226974'-Chloropropiophenone

生成物 1

HCID 54270636HCID 54270636、化合物収率 94.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

13.47 g of chlorotrimethylsilane are slowly added to 12.55 g of triethylamine, under a nitrogen atmosphere, at 20°±3° C. 16.86 g of 4-chloropropiophenone (endothermic mixture) and then a solution of 18.58 g of sodium iodide in 125 ml of acetonitrile are further added while maintaining the temperature at 18°±2° C. The mixture is then heated for 3 hours at 40°±5° C., the acetonitrile is removed under reduced pressure and 150 ml of toluene are added to the solid residue. 50 ml of solvent are distilled under reduced pressure to drive the residual acetonitrile off. The inorganic materials are extracted with 100 ml of iced water, the organic phase is washed with 100 ml of iced water and dried over magnesium sulfate. The toluene is removed under reduced pressure and complete removal of the solvents is performed for 15 hours at 60° C. under a pressure of 1 mbar to give 22.7 g of an oil. NMR run at 200 MHz (CDCl3) 0.13 ppm:s:9H 1.7 ppm:d:3H 5.28 ppm:q:1H 7.21-7.39 ppm:m:4H.

後処理

  1. temperaturewhile maintaining the temperature at 18°±2° C
  2. temperatureThe mixture is then heated for 3 hours at 40°±5° C.
  3. customthe acetonitrile is removed under reduced pressure and 150 ml of toluene
  4. additionare added to the solid residue
  5. distillation50 ml of solvent are distilled under reduced pressure
  6. extractionThe inorganic materials are extracted with 100 ml of iced water
  7. washthe organic phase is washed with 100 ml of iced water
  8. dry with materialdried over magnesium sulfate
  9. customThe toluene is removed under reduced pressure and complete removal of the solvents

出典と根拠

ORDレコード
ord-4bb16c8d9f9f401b9162ef6f15f74ee4
出典データセット
uspto-grants-1997_04
特許番号
US05624941

関連ノート

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