Hydrochloric Acid → HCID 53985323、化合物

HRID 2219226ノート

反応式

HRID 2219226 の反応式
Cl.C([O:4][CH:5](OCC)[CH2:6][O:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1)C>CCOCC>[C:12]([C:11]1[CH:14]=[CH:15][C:8]([O:7][CH2:6][CH:5]=[O:4])=[CH:9][CH:10]=1)#[N:13]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 177499644-(2,2-Diethoxyethoxy)benzonitrile

生成物 1

HCID 53985323HCID 53985323、化合物収率 99.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A 5N HCl (25 mL) solution is added to a stirred solution of 4-(2,2-diethoxy-ethoxy)-benzonitrile (2.00 g, 8.50 mmol) in Et2O (25 mL). The two-layered solution is stirred vigorously at ambient temperature under nitrogen for 24 hours. Another 50 mL Et2O is added to the mixture. The organic layer is separated, washed with an aqueous solution (30 mL) containing saturated NaHCO3 (0.5 mL), dried over MgSO4, filtered and concentrated at ambient temperature to give 1.36 g of the crude (4-cyano-phenoxy)acetaldehyde as oil. The oil is diluted in Et2O to form a stock solution (25 mg/mL), which is used for the subsequent reaction. 1H NM (CDCl3): δ4.66 (s, 2H), 9.85 (s, 1H).

後処理

  1. customThe organic layer is separated
  2. washwashed with an aqueous solution (30 mL)
  3. additioncontaining saturated NaHCO3 (0.5 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated at ambient temperature

出典と根拠

ORDレコード
ord-e5a412107ada495a82126dcd886af2b8
出典データセット
uspto-grants-2008_08
特許番号
US07414063B2

反応ノート

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