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Hydrochloric Acid → ST51001684

HRID 2308577
ノート
印刷プレビュー

反応式

HRID 2308577 の反応式
[Na].C(OCC)(=O)[CH2:3][C:4](OCC)=[O:5].[CH2:13]([S:15][CH:16]([CH3:23])[CH2:17][CH:18]=[CH:19][C:20](=[O:22])[CH3:21])[CH3:14].[OH-].[Na+].Cl>O.C(O)C>[CH2:13]([S:15][CH:16]([CH3:23])[CH2:17][CH:18]1[CH2:3][C:4](=[O:5])[CH2:21][C:20](=[O:22])[CH2:19]1)[CH3:14]
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

8

反応物 5

HCID 313Hydrochloric AcidHCID 7761Diethyl MalonateHCID 14798Sodium Hydroxide2 回HCID 5360545SodiumHCID 544576116-Ethylthio-3-hepten-2-one

生成物 1

HCID 3116068ST51001684

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

2.53 g of metallic sodium were added to 100 ml of ethanol at room temperature. To this was then added 17.6 g of diethyl malonate, with stirring, and then 17.2 g of 6-ethylthio-3-hepten-2-one was added. The resulting mixture was then refluxed for four hours and then an aqueous sodium hydroxide solution, containing 9.5 g of sodium hydroxide in 75 ml of water, was added and the mixture refluxed for another two hours. The mixture was cooled to 50° C. and then acidified by the addition of concentrated hydrochloric acid. The mixture was then warm until decarboxylation was complete and then evaporated to a liquid residue. The residue was mixed with ethyl ether, washed with water, and evaporated to a brown liquid. The liquid was base, acid extracted affording 5-(2-ethylthiopropyl) cyclohexane-1,3-dione.

後処理

  1. temperatureThe resulting mixture was then refluxed for four hours
  2. additionwas added
  3. temperaturethe mixture refluxed for another two hours
  4. temperatureThe mixture was then warm until decarboxylation
  5. customevaporated to a liquid residue
  6. additionThe residue was mixed with ethyl ether
  7. washwashed with water
  8. customevaporated to a brown liquid
  9. extractionextracted

出典と根拠

ORDレコード
ord-ff366789a4984be2945e267db2899630
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE032489

反応ノート

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