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Hydrochloric Acid → HCID 58043122、化合物

HRID 1035214
ノート
印刷プレビュー

反応式

HRID 1035214 の反応式
[CH3:1][O:2][C:3]1[C:10]([CH3:11])=[C:9]([O:12]C2CCCCO2)[CH:8]=[CH:7][C:4]=1[CH:5]=[O:6].Cl>C(O)C>[OH:12][C:9]1[CH:8]=[CH:7][C:4]([CH:5]=[O:6])=[C:3]([O:2][CH3:1])[C:10]=1[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 107531772-Methoxy-3-methyl-4-(tetrahydro-2H-pyran-2-yloxy)benzaldehyde

生成物 1

HCID 58043122HCID 58043122、化合物収率 72%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Methoxy-3-methyl-4-(tetrahydro-2H-pyran-2-yloxy)benzaldehyde—for preparation see e.g. Journal of Medicinal Chemistry, 41, 4819-4832 (1998)—(2.10 g, 8.4 mmol) was dissolved in ethanol (40 mL) and then HCl (2M, 40 mL) was added. After 20 minutes the solution was concentrated under reduced pressure. The aqueous residue was extracted twice with EtOAc and the combined organic solutions were washed with brine. The solution was dried over Na2SO4 and the solvent was removed by evaporation. The product was washed with petroleum-ether. There was obtained 1.0 g (72%) of 52A as a solid. 1H NMR (500 MHz, CDCl3): δ 2.05 (s, 3H), 3.78 (s, 3H), 6.74 (d, 1H), 7.49 (d, 1H), 10.05 (s, 1H).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationAfter 20 minutes the solution was concentrated under reduced pressure
  2. extractionThe aqueous residue was extracted twice with EtOAc
  3. washthe combined organic solutions were washed with brine
  4. dry with materialThe solution was dried over Na2SO4
  5. customthe solvent was removed by evaporation
  6. washThe product was washed with petroleum-ether

出典と根拠

ORDレコード
ord-f0adf8ecca024ebea9c7bbd4238d8e18
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546375B2

反応ノート

読み込み中…