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Hydrochloric Acid → HCID 11984309, 화합물

HRID 493463
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HRID 493463 반응식
[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]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 11984308HCID 11984308, 화합물

생성물 1

HCID 11984309HCID 11984309, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 3283
Diethyl Ether
용매

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온도
70 °C

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-d99f797bfdbf4b60bf9cf2502077d058
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07534908B2

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