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Sodium Iodide → HCID 21317518、化合物

HRID 328764
ノート
印刷プレビュー

反応式

HRID 328764 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 131047161-Chloro-4-acetoxynonane

生成物 1

HCID 21317518HCID 21317518、化合物収率 98%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6bc823adb9dc4e04a430467a72d41239
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04018802

反応ノート

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