Sodium Iodide → HCID 13046305, 화합물

HRID 328829노트

반응식

HRID 328829 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 13046305HCID 13046305, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-359d5a221a86478080bbb0c6d9da03e3
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018811

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