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Hydrochloric Acid → HCID 11984309、化合物

HRID 493463
ノート
印刷プレビュー

反応式

HRID 493463 の反応式
[OH-].[Na+].CO.[CH3:5][C@@H:6]([CH:11]([C:17]([O:19]CC)=[O:18])[C:12]([O:14]CC)=[O:13])[CH2:7][CH2:8][CH2:9][CH3:10].Cl>O.CCOCC>[CH3:5][C@@H:6]([CH:11]([C:17]([OH:19])=[O:18])[C:12]([OH:14])=[O:13])[CH2:7][CH2:8][CH2:9][CH3:10]
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

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 11984308HCID 11984308、化合物

生成物 1

HCID 11984309HCID 11984309、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether
溶媒

反応条件

温度
70 °C

実験手順

At room temperature, 81 g of sodium hydroxide (2 mol) were dissolved in 360 ml of water and 160 ml of methanol in a three-neck flask with internal thermometer, dropping funnel and stirrer. 124 g of diethyl [(R)-1-methylpentyl]malonate (0.51 mol) were then added. The mixture was heated to 70° C. and stirred at this temperature for 3.5 h, in the course of which a solid formed. After cooling to 25° C., the suspension was admixed with 250 ml of ether and, with cooling, with 400 ml of 20% by weight hydrochloric acid. After phase separation, the aqueous phase was extracted twice with 100 ml of ether. The combined organic phases were washed with 100 ml of water and then dried over sodium sulfate. After solvent had been distilled off, [(R)-1-methylpentyl]malonic acid was obtained in a yield of 85 g (89% of theory) (m.p.: 123° C.).

後処理

  1. customformed
  2. temperatureAfter cooling to 25° C.
  3. customAfter phase separation
  4. extractionthe aqueous phase was extracted twice with 100 ml of ether
  5. washThe combined organic phases were washed with 100 ml of water
  6. dry with materialdried over sodium sulfate
  7. distillationAfter solvent had been distilled off

出典と根拠

ORDレコード
ord-d99f797bfdbf4b60bf9cf2502077d058
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07534908B2

反応ノート

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