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Sodium Iodide → Iodomethyl 2-ethylbutanoate

HRID 1712887
ノート
印刷プレビュー

反応式

HRID 1712887 の反応式
Cl[CH2:2][O:3][C:4](=[O:10])[CH:5]([CH2:8][CH3:9])[CH2:6][CH3:7].[I-:11].[Na+].COC(C)(C)C.S([O-])([O-])(=O)=S.[Na+].[Na+]>CC(C)=O>[I:11][CH2:2][O:3][C:4](=[O:10])[CH:5]([CH2:8][CH3:9])[CH2:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 15413tert-Butyl methyl etherHCID 24477Sodium ThiosulfateHCID 13138744Chloromethyl 2-ethylbutyrate

生成物 1

HCID 23449337Iodomethyl 2-ethylbutanoate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2-Ethyl butyric acid chloromethyl ester (700 g) was dissolved in acetone (3 L). To this solution was added sodium iodide (1.0 kg). The resulting reaction mixture was heated at reflux until reaction completion (2 h (hours), monitored by GC). The solution was then cooled to ambient temperature where tert-butyl methyl ether (7 L) and 5% aqueous sodium thiosulfate (4 L) were added. The phases were separated and the organic phase was washed with aqueous sodium thiosulfate (4 L), low pyrogen water (4 L) and 10% sodium chloride solution (4 L). The organic layer was dried over magnesium sulfate (350 g), filtered, and the filter cake was washed with tert-butyl methyl ether (2×0.7 L). The filtrate was evaporated to a small volume (ca. 2 L) to give 2-ethyl butyric acid iodomethyl ester, as a solution in tert-butyl methyl ether.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureat reflux until reaction completion (2 h (hours), monitored by GC)
  4. additionwere added
  5. customThe phases were separated
  6. washthe organic phase was washed with aqueous sodium thiosulfate (4 L), low pyrogen water (4 L) and 10% sodium chloride solution (4 L)
  7. dry with materialThe organic layer was dried over magnesium sulfate (350 g)
  8. filtrationfiltered
  9. washthe filter cake was washed with tert-butyl methyl ether (2×0.7 L)
  10. customThe filtrate was evaporated to a small volume (ca. 2 L)

出典と根拠

ORDレコード
ord-3e823e68f19f45f29bf535b2518ebd6a
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795243B2

反応ノート

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