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Ethyl benzoylacetate → 14895-21-7

HRID 2394000
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HRID 2394000 반응식
[C:1]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](=[O:18])(O)[O-].[Na+]>ClC1C=CC=CC=1Cl>[C:1]([C:9]1[C:10](=[O:11])[O:12][C:13]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:14][C:15]=1[OH:18])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7170Ethyl benzoylacetateHCID 516892Sodium Bicarbonate

생성물 1

HCID 13544742214895-21-7

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

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온도
0 °C

실험 절차

To a solution of ethyl benzoylacetate (150 g, 0.88 mmol) in 1,2-dichlorobenzene (150 mL) was added a trace amount of sodium bicarbonate. The reaction mixture was heated to reflux. A distillate of ethanol (approximately 20 mL) was collected. The reaction mixture was cooled to 0° C. Ether (100 mL) was added to induce crystallization. The reaction mixture was kept in the refrigerator overnight. The solid formed was collected and washed with ether: m.p. 171°-173° C.; 1H NMR (250 MHz, DMSO-d6) δ 6.91 (s, 1 H), 7.59 (m, 6 H), 7.87 (m, 4 H).

후처리

  1. temperatureThe reaction mixture was heated to reflux
  2. distillationA distillate of ethanol (approximately 20 mL) was collected
  3. additionEther (100 mL) was added
  4. customcrystallization
  5. customwas kept in the refrigerator overnight
  6. customThe solid formed
  7. customwas collected
  8. washwashed with ether

출처 및 근거

ORD 기록
ord-baf05ccac4dc4d3c8482f62b24524231
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05808062

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