(3-(Benzyloxy)phenyl)hydrazine hydrochloride → HCID 118497040, 화합물

HRID 522153노트

반응식

HRID 522153 반응식
[C:1](/[CH:3]=[C:4](\[O-])/[C:5]([O:7][CH2:8][CH3:9])=[O:6])#[N:2].[K+].Cl.[CH2:13]([O:20][C:21]1[CH:22]=[C:23]([NH:27][NH2:28])[CH:24]=[CH:25][CH:26]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[NH2:2][C:1]1[N:27]([C:23]2[CH:24]=[CH:25][CH:26]=[C:21]([O:20][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH:22]=2)[N:28]=[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH:3]=1

참가 물질

4

반응물 2

HCID 12891839(3-(Benzyloxy)phenyl)hydrazine hydrochlorideHCID 20619185Potassium 1-cyano-3-ethoxy-3-oxoprop-1-en-2-olate

생성물 1

HCID 118497040HCID 118497040, 화합물수율 68%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of potassium (Z)-1-cyano-3-ethoxy-3-oxoprop-1-en-2-olate (3.73 g, 20.82 mmol) in ethanol (100 mL) was added (3-(benzyloxy)phenyl)hydrazine hydrochloride (Preparation 61, 5.22 g, 20.82 mmol) and the reaction was heated at reflux for 24 hours. The reaction was cooled to room temperature, the solid was filtered and the filtrate was concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 20-40% EtOAc in heptanes to afford the title compound (4.76 g, 68%).

후처리

  1. temperaturethe reaction was heated
  2. temperatureat reflux for 24 hours
  3. filtrationthe solid was filtered
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe residue was purified
  6. washeluting with 20-40% EtOAc in heptanes

출처 및 근거

ORD 기록
ord-323b9740eee740beb221ff9e552b5e5d
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328096B2

반응 노트

불러오는 중…