Sodium Iodide → HCID 20320776、化合物

HRID 866392ノート

反応式

HRID 866392 の反応式
Cl/[CH:2]=[CH:3]/[C:4]([CH:6]1[CH2:9][C:8]2([CH2:12][CH2:11][CH2:10]2)[CH2:7]1)=[O:5].[I-:13].[Na+]>CC(C)=O>[I:13]/[CH:2]=[CH:3]/[C:4]([CH:6]1[CH2:9][C:8]2([CH2:12][CH2:11][CH2:10]2)[CH2:7]1)=[O:5]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 203207682-Propen-1-one, 3-chloro-1-spiro[3.3]hept-2-yl-, (E)-

生成物 1

HCID 20320776HCID 20320776、化合物収率 62.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

1-Chloro-3-(spiro[3.3]hept-2-yl)-1E-propen-3-one (7.3 g, 0.042 mole) was mixed with 25.2 g (0.168 mole) of sodium iodide and 45 ml of dry acetone (distilled from anhydrous potassium carbonate, b.p. 56° C). The mixture was refluxed with rapid stirring overnight. The mixture was cooled and the solvent was removed in vacuo. The solid residue was taken up in 75 ml of water and the products were extracted with 150 ml (3×50 ml) of ether. The organic material was washed with 50 ml of saturated sodium bicarbonate solution, 50 ml of aqueous sodium thiosulfate solution and 50 ml of saturated sodium chloride solution. The material was dried over anhydrous magnesium sulfate, filtered and the solvent was removed in vacuo to yield 6.9 g (62.2%) of crude 1-iodo-3-(spiro[3.3]hept-2-yl)-1E-propen-3-one.

後処理

  1. temperatureThe mixture was refluxed
  2. temperatureThe mixture was cooled
  3. customthe solvent was removed in vacuo
  4. extractionthe products were extracted with 150 ml (3×50 ml) of ether
  5. washThe organic material was washed with 50 ml of saturated sodium bicarbonate solution, 50 ml of aqueous sodium thiosulfate solution and 50 ml of saturated sodium chloride solution
  6. dry with materialThe material was dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-f0b7d444b87a476792deff1346e53b79
出典データセット
uspto-grants-1978_07
特許番号
US04098823

反応ノート

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