Hydrochloric Acid → HCID 53985323, 화합물

HRID 2219226노트

반응식

HRID 2219226 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 53985323HCID 53985323, 화합물수율 99.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e5a412107ada495a82126dcd886af2b8
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07414063B2

반응 노트

불러오는 중…