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Acetic Acid → HCID 68154567, 화합물

HRID 1615733
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HRID 1615733 반응식
CC(C)([O-])C.[Na+].[CH2:7]([O:9][C:10]([CH2:12][O:13][CH2:14][CH2:15][O:16][CH2:17][C:18]([O:20]CC)=O)=[O:11])[CH3:8].C(O)(=O)C>C1COCC1>[O:20]=[C:18]1[CH2:17][O:16][CH2:15][CH2:14][O:13][CH:12]1[C:10]([O:9][CH2:7][CH3:8])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 13237171Diethyl 2,2'-(ethane-1,2-diylbis(oxy))diacetateHCID 23676156Sodium t-butoxide

생성물 1

HCID 68154567HCID 68154567, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The mixing was carried out under a protective nitrogen gas atmosphere. 7.93 g (80.0 mmol) sodium-tert-butoxide were placed in 150 ml THF and heated to boiling point. At this temperature 8.50 g (36.3 mmol) ethyl (2-ethoxycarbonylmethoxy-ethoxy)-acetate (prepared analogously to Canadian Journal of Chemistry; 74; 8; 1996; 1437-1446) in 100 ml THF were added dropwise within 3 h. After the addition had ended the mixture was refluxed for 1 h and then stirred overnight at RT. Then the reaction mixture was adjusted to pH 5 with glacial acetic acid and concentrated by rotary evaporation. The residue was mixed with water and extracted with ethyl acetate. The organic phases were combined, dried and the solvent was eliminated under reduced pressure and with gentle heating.

후처리

  1. temperatureheated
  2. additionAfter the addition
  3. temperaturewas refluxed for 1 h
  4. concentrationconcentrated by rotary evaporation
  5. additionThe residue was mixed with water
  6. extractionextracted with ethyl acetate
  7. customdried

출처 및 근거

ORD 기록
ord-6942a0b85eb34e349f9724834d555e26
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765763B2

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