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Methanol → HCID 89649130, 화합물

HRID 2207652
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HRID 2207652 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[CH:6][C:7]([F:21])=[C:8]([C:10]2[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[N:13]=[C:12]([C:19]#N)[CH:11]=2)[CH:9]=1)[CH3:2].[O:22]1CCOC[CH2:23]1.C[OH:29]>Cl>[CH2:1]([O:3][C:4]1[CH:5]=[CH:6][C:7]([F:21])=[C:8]([C:10]2[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[N:13]=[C:12]([C:19]([O:22][CH3:23])=[O:29])[CH:11]=2)[CH:9]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 312751,4-DioxaneHCID 89649694HCID 89649694, 화합물

생성물 1

HCID 89649130HCID 89649130, 화합물

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A mixture of 4-(5-ethoxy-2-fluoro-phenyl)-6-isopropyl-pyridine-2-carbonitrile (which may be prepared as described in Description 114) (1.09 g, 3.8 mmol) in 4M HCl in dioxan (12 mL, 48 mmol) and methanol (12 mL) was heated to reflux under nitrogen overnight. The solvents were evaporated and ethyl acetate (150 ml) and NaHCO3 solution (150 ml) were added. The product was extracted into ethyl acetate (3 x) and the extracts were dried (Na2SO4) and concentrated. Chromatography (0-10% diethyl ether in DCM) gave methyl 4-(5-ethoxy-2-fluoro-phenyl)-6-isopropyl-pyridine-2-carboxylate (D115) (730.8 mg);

후처리

  1. temperatureto reflux under nitrogen overnight
  2. customThe solvents were evaporated
  3. additionethyl acetate (150 ml) and NaHCO3 solution (150 ml) were added
  4. extractionThe product was extracted into ethyl acetate (3 x)
  5. dry with materialthe extracts were dried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ea90dda6b5a943e5b7bcc1d48daf201a
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376436B2

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