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Diethyl Ether → [3-(Hex-5-en-1-yl)oxiran-2-yl]methanol

HRID 622861
ノート
印刷プレビュー

反応式

HRID 622861 の反応式
[CH2:1]([OH:10])/[CH:2]=[CH:3]/[CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9].C([O:15]O)(C)(C)C.S([O-])([O-])(=O)=O.[Na+].[Na+].C(OCC)C>C1(C)C=CC=CC=1>[O:15]1[CH:3]([CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9])[CH:2]1[CH2:1][OH:10]
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 3283Diethyl EtherHCID 6410tert-Butyl hydroperoxideHCID 24436Sodium SulfateHCID 14152343HCID 14152343、化合物

生成物 1

HCID 14152344[3-(Hex-5-en-1-yl)oxiran-2-yl]methanol収率 82%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

2.72 g (19.4 mM) (E)-nona-2,8-diene-1-ol (11) is added into the reaction mixture after another 5 minutes. Then, after yet another 5 minutes, 6.9 ml of a 3.39 molar solution in toluene (23.4 mM) of tertiary butyl hydroperoxide is added. The reaction mixture is allowed to react for 3 days at -25° C. Subsequently, the reaction vessel is put into an ice bath and 10 ml (1 ml per mM tetraisopropyl titantate added) saturated aqueous sodium sulfate solution and another 100 ml diethyl ether are added to the reaction mixture. The reaction solution is vigorously agitated for approximately 1 hour until the solution has warmed up to room temperature. The gelatinous orange-colored precipitation is separated out by means of a glass filter, washed twice with 100 ml quantities of ether and dried by suction. The solvent is evaporated from the combined filtrates and the residue is mixed with 100 ml ether and 2 ml dimethyl sulfide in order to destroy excess tertiary butyl hydroperoxide. The solution is agitated for one hour. Then, 50 ml 1 molar sodium hydroxide is added and the mixture is agitated another 3-4 hours. The ether phase is separated out, washed with 2×40 ml water, dried over magnesium sulfate and, after evaporation of the solvent in a vacuum, 2.48 g (15.9 mM) 2S, 3S-2-epoxy-1-hydroxynon-8-ene (III) is obtained by bulb tube distillation at 110° C./0.5 mm pressure. This corresponds to a yield of 82%.

後処理

  1. customto react for 3 days at -25° C
  2. customSubsequently, the reaction vessel is put into an ice bath
  3. customThe gelatinous orange-colored precipitation
  4. customis separated out by means of a glass
  5. filtrationfilter
  6. washwashed twice with 100 ml quantities of ether
  7. customdried by suction
  8. customThe solvent is evaporated from the combined filtrates
  9. additionthe residue is mixed with 100 ml ether and 2 ml dimethyl sulfide in order
  10. customto destroy excess tertiary butyl hydroperoxide
  11. stirringThe solution is agitated for one hour
  12. additionThen, 50 ml 1 molar sodium hydroxide is added
  13. stirringthe mixture is agitated another 3-4 hours
  14. customThe ether phase is separated out
  15. washwashed with 2×40 ml water
  16. dry with materialdried over magnesium sulfate
  17. customafter evaporation of the solvent in a vacuum, 2.48 g (15.9 mM) 2S

出典と根拠

ORDレコード
ord-612c4d139b504c18a80ab8ebe33c9d34
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04772727

反応ノート

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