Hydrazine hydrate (1:1) → 4-Cyanobenzohydrazide

HRID 563214

반응식

HRID 563214 반응식
[C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7](OCC)=[O:8])=[CH:5][CH:4]=1)#[N:2].O.[NH2:15][NH2:16]>C(O)C>[C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7]([NH:15][NH2:16])=[O:8])=[CH:5][CH:4]=1)#[N:2]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 81589Ethyl 4-cyanobenzoate

생성물 1

HCID 4567324-Cyanobenzohydrazide수율 90.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a 250 mL round bottom flask charged with ethyl 4-cyanobenzoate (16.85 g, 96.2 mmol) in 95% ethanol (75 mL) was added hydrazine mono-hydrate (18.2 mL, 64% solution, 240 mmol). This mixture was heated to reflux for a period of 4.5 h, then allowed to cool to room temperature over a 16 h period. The solvent was removed under reduced pressure and the yellow residue was taken up in ice-cold water (150 mL). The light yellow solid was filtered off and washed with additional cold water (50 mL). The solid was then dried under high vacuum to yield the title compound as a light yellow solid (13.98 g, 90%). 1H NMR (400 MHz, DMSO-d6, δ in ppm) 10.05 (br s, 1H), 7.95 (AA′XX′, J=8.5 Hz, 4H), 4.61 (br s, 2H).

후처리

  1. temperatureThis mixture was heated
  2. temperatureto reflux for a period of 4.5 h
  3. customThe solvent was removed under reduced pressure
  4. filtrationThe light yellow solid was filtered off
  5. washwashed with additional cold water (50 mL)
  6. customThe solid was then dried under high vacuum

출처 및 근거

ORD 기록
ord-1e5e5ec393cf42a99f134be34ad05bff
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067448B2

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