Sodium Iodide → HCID 54270636, 화합물

HRID 55364

반응식

HRID 55364 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 54270636HCID 54270636, 화합물수율 94.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4bb16c8d9f9f401b9162ef6f15f74ee4
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624941

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