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Hydrochloric Acid → HCID 13946785、化合物

HRID 1863524
ノート
印刷プレビュー

反応式

HRID 1863524 の反応式
COC([CH:5]1[CH:9]([CH:10]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[CH:11]=[CH:12]/[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:8][O:7][C:6]1=[O:25])=O.[Cl-].[Li+].Cl>CN(C)P(=O)(N(C)C)N(C)C>[C:19]1([S:18][CH:10]([CH:9]2[CH2:8][O:7][C:6](=[O:25])[CH2:5]2)/[CH:11]=[CH:12]/[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 433294Lithium ChlorideHCID 20392009HCID 20392009、化合物

生成物 1

HCID 13946785HCID 13946785、化合物

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

反応条件

温度
100 °C

実験手順

60 mg (0.17 mmol) of 3-methoxycarbonyl-4-(1-phenylthio-trans-2-octenyl)-oxolane-2-one was dissolved in 2 ml of hexamethyl phosphoric triamide in an argon atmosphere, and 36 mg (0.85 mmol) of lithium chloride was added to the solution followed by heating at a temperature of 100° C. for 5 hours with stirring. The reaction mixture was then allowed to cool to room temperature and decomposed with dilute hydrochloric acid. The mixture was extracted with ethyl acetate, and the extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrated was concentrated under reduced pressure. The resulting residue was then purified by silica gel column chromatography to obtain 4-(1-phenylthio-trans-2-octenyl)-oxolane-2-one.

後処理

  1. additionwas added to the solution
  2. temperatureto cool to room temperature
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe extract was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationThe mixture was filtered
  7. concentrationthe filtrated was concentrated under reduced pressure
  8. customThe resulting residue was then purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-72a5f5b514a5431ea64686ad37628917
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04169199

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート