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Sodium Iodide → HCID 21317518, 화합물

HRID 2083280
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HRID 2083280 반응식
Cl[CH2:2][CH2:3][CH2:4][CH:5]([O:11][C:12](=[O:14])[CH3:13])[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[I-:15].[Na+]>CC(C)=O>[I:15][CH2:2][CH2:3][CH2:4][CH:5]([O:11][C:12](=[O:14])[CH3:13])[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
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참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 131047161-Chloro-4-acetoxynonane

생성물 1

HCID 21317518HCID 21317518, 화합물수율 98%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 1-chloro-4-acetoxynonane (Ex. 1, Step B-3) (35.3 g., 0.16 mole) and sodium iodide (120 g., 0.8 mole) in acetone (350 ml.) is stirred and heated at reflux with exclusion of light for 10 hours. The resulting suspension is filtered and the collected sodium chloride washed with acetone. The combined filtrate and washings are evaporated in vacuo leaving a residual mass which is partitioned between ether and water. The organic extract is washed with dilute aqueous sodium thiosulfate and water, dried over sodium sulfate and evaporated in vacuo providing the title compound as a colorless liquid (48.7 g., 98%), pmr (CDCl3) δ 2.0 (s, 3H), 3.18 (t, 2H) and 4.98 (m, H).

후처리

  1. temperatureheated
  2. temperatureat reflux with exclusion of light for 10 hours
  3. filtrationThe resulting suspension is filtered
  4. washthe collected sodium chloride washed with acetone
  5. customThe combined filtrate and washings are evaporated in vacuo
  6. customleaving a residual mass which
  7. customis partitioned between ether and water
  8. extractionThe organic extract
  9. washis washed with dilute aqueous sodium thiosulfate and water
  10. dry with materialdried over sodium sulfate
  11. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-197bd306ffef4dec96c4599681598e19
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04085125

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