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5-(Isopropyl)cyclohexane-1,3-dione → HCID 178439430, 화합물

HRID 485606
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HRID 485606 반응식
C(O[C:4]1[CH2:8][CH2:7][CH2:6][N:5]=1)C.[CH3:9][CH:10]([CH:12]1[CH2:17][C:16](=[O:18])[CH2:15][C:14](=[O:19])[CH2:13]1)[CH3:11]>C(O)(C)C>[CH3:11][CH:10]([CH:12]1[CH2:13][C:14](=[O:19])[C:15](=[C:4]2[CH2:8][CH2:7][CH2:6][NH:5]2)[C:16](=[O:18])[CH2:17]1)[CH3:9]
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참가 물질

4

반응물 2

HCID 5661065-(Isopropyl)cyclohexane-1,3-dioneHCID 109861852-Ethoxy-1-pyrroline

생성물 1

HCID 178439430HCID 178439430, 화합물수율 12.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 2-ethoxy-1-pyrroline (9.05 grams, 0.08 mole), and 5-(1-methylethyl)-1,3-cyclohexanedione (12.34 grams, 0.08 mole), in 50 mL of isopropyl alcohol solvent is heated under reflux for 2 hours. After standing overnight, the cooled reaction solution will deposit white, crystalline product which is collected, washed with cold solvent and dried to give 2.2 grams of solid, m.p. 143°-145° C. The filtrate is evaporated and the residue dissolved in dichloromethane and the solution extracted with three portions of 3N NaOH followed by three portions of 3N hydrochloric acid. Addition of 3N NaOH to the acid solution causes precipitation of an 0.87-gram portion of product, m.p. 143.5°-145° C. The latter is recrystallized from ethyl acetate for an analytical sample.

후처리

  1. temperatureunder reflux for 2 hours
  2. customthe cooled reaction solution
  3. customcrystalline product which is collected
  4. washwashed with cold solvent
  5. customdried

출처 및 근거

ORD 기록
ord-33572bd5866e4a1996ad253b0ea8e0e3
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04537616

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