(3-(Benzyloxy)phenyl)hydrazine hydrochloride → HCID 118497040、化合物

HRID 522153ノート

反応式

HRID 522153 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 118497040HCID 118497040、化合物収率 68%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-323b9740eee740beb221ff9e552b5e5d
出典データセット
uspto-grants-2016_05
特許番号
US09328096B2

反応ノート

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