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Hydrochloric Acid → HCID 11636865、化合物

HRID 2249663
ノート
印刷プレビュー

反応式

HRID 2249663 の反応式
[CH3:1][CH:2]([CH3:15])[CH2:3][CH:4]=[C:5]1[CH2:14][CH2:13][C:8]2(OCC[O:9]2)[CH2:7][CH2:6]1.Cl.C(Cl)(Cl)Cl.O>O1CCCC1>[CH3:1][CH:2]([CH3:15])[CH2:3][CH:4]=[C:5]1[CH2:6][CH2:7][C:8](=[O:9])[CH2:13][CH2:14]1
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 313Hydrochloric AcidHCID 962WaterHCID 6212ChloroformHCID 689871908-(3-Methylbutylidene)-1,4-dioxaspiro[4.5]decane

生成物 1

HCID 11636865HCID 11636865、化合物収率 83.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In 50 ml of tetrahydrofuran is dissolved 10.0 g of 8-(3-methylbutylidene)-1,4-dioxaspiro[4.5]decane. After adding 50 ml of 6 mol/L hydrochloric acid, the mixture thus obtained is stirred at ambient temperature for one hour. Chloroform and water are added to the reaction mixture and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=98:2) to obtain 6.6 g of 4-(3-methylbutylidene)-1-cyclohexanone as a colorless oily product.

後処理

  1. customthe mixture thus obtained
  2. customthe organic layer is separated
  3. customThe organic layer thus obtained
  4. washis washed with water and saturated aqueous solution of sodium chloride successively
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent is distilled off under reduced pressure
  7. customThe residue thus obtained
  8. customis purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=98:2)

出典と根拠

ORDレコード
ord-f5ba0ed274ca4c4baca604f6cc045e3b
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

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