Sodium Iodide → HCID 13046305、化合物

HRID 442087ノート

反応式

HRID 442087 の反応式
[CH3:1][C:2]([CH3:14])([CH2:9][CH2:10][CH2:11][CH2:12]Cl)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[I-:15].[Na+]>C(C(C)=O)C>[CH3:1][C:2]([CH3:14])([CH2:9][CH2:10][CH2:11][CH2:12][I:15])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 21767804Ethyl 3,3-dimethyl-7-chloroheptanoate

生成物 1

HCID 13046305HCID 13046305、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

To a solution of 3.57 g. (0.0162 mole) of ethyl 3,3-dimethyl-7-chloroheptanoate in 100 ml. of methyl ethyl ketone is added 4 g. of sodium iodide and the mixture heated at reflux for 18 hours. The reaction mixture is cooled, filtered and concentrated. The residue is partitioned between ether and water. The aqueous phase is extracted several times with ether. The extract is washed with sodium bisulfite solution, water and saline. The organic solution is dried over magnesium sulfate and concentrated to give 4.182 g. of a yellow oil. The material is purified by distillation, b.p. 86°-87° C. (0.18 Torr).

後処理

  1. temperatureat reflux for 18 hours
  2. temperatureThe reaction mixture is cooled
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue is partitioned between ether and water
  6. extractionThe aqueous phase is extracted several times with ether
  7. washThe extract is washed with sodium bisulfite solution, water and saline
  8. dry with materialThe organic solution is dried over magnesium sulfate
  9. concentrationconcentrated
  10. customto give 4.182 g
  11. distillationThe material is purified by distillation, b.p. 86°-87° C. (0.18 Torr)

出典と根拠

ORDレコード
ord-eac82357a45b45969f486c86ae69b446
出典データセット
uspto-grants-1977_08
特許番号
US04044043

反応ノート

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