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Propionic Acid → HCID 67330102, 화합물

HRID 2408243
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HRID 2408243 반응식
[C:1](OC)([O:5][CH3:6])([O:3]C)[CH3:2].[C:9]1([CH:15](O)[C:16]([CH3:18])=[CH2:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(O)(=O)CC>CO>[CH3:17]/[C:16](=[CH:15]\[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)/[CH2:18][CH2:2][C:1]([O:5][CH3:6])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1032Propionic AcidHCID 15050Trimethyl orthoacetateHCID 1382112-Methyl-1-phenyl-2-propen-1-ol

생성물 1

HCID 67330102HCID 67330102, 화합물수율 21%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Trimethyl orthoacetate (186 g, 1.52 mol) and 1-phenyl-2-methyl-2-propen-1-ol (90% pure from Alfa Aesar, 25 g, 0.152 mol) were heated in the presence of propionic acid (0.2 ml) in an oil bath at 145° C. for 4 hours. The methanol formed during the reaction was distilled. The excess orthoacetate was then removed under vacuum and the residue was purified by column chromatography on silica gel (eluent: heptanes/ethyl acetate 25:1 to 8:1) followed by bulb-to-bulb distillation (67° C./0.001 mbar). 6.5 g (yield=21%) of the desired product were obtained.

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후처리

  1. distillationwas distilled
  2. customThe excess orthoacetate was then removed under vacuum
  3. customthe residue was purified by column chromatography on silica gel (eluent: heptanes/ethyl acetate 25:1 to 8:1)
  4. distillationfollowed by bulb-to-bulb distillation (67° C./0.001 mbar)

출처 및 근거

ORD 기록
ord-d30270d395fc49209f089ff6d6301b15
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815792B2

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