HCID 86677027、化合物 → HCID 178435906、化合物

HRID 927174ノート

反応式

HRID 927174 の反応式
OC1C(=O)NN=C(CCC2C=CC=CC=2)C=1.C([O:24][C:25]1[N:26]=[N:27][C:28]([C:39]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[CH2:40])=[CH:29][C:30]=1[O:31]CC1C=CC=CC=1)C1C=CC=CC=1>C(OCC)(=O)C>[C:41]1([CH:39]([C:28]2[CH:29]=[C:30]([OH:31])[C:25](=[O:24])[NH:26][N:27]=2)[CH3:40])[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1

参加物

4

反応物 2

HCID 86677027HCID 86677027、化合物2 回HCID 1785188083-Hydroxy-6-(2-Phenylethyl)pyridazin-4(1h)-One

生成物 1

HCID 178435906HCID 178435906、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Prepared by the same method as for 4-hydroxy-6-(2-phenylethyl)pyridazin-3(2H)-one (Example 1) from 3,4-bis(benzyloxy)-6-(1-phenylethenyl)pyridazine (Intermediate 25) except that upon completion of the reaction the resulting mixture was filtered through Celite washing with ethanol and then concentrated in vacuo to afford an orange solid. This was purified initially by eluting on a reverse phase C18 chromatography column (0-60% methanol in water with an acidic modifier) and upon combining and concentrating the appropriate fractions the crude product was recrystallised from a mixture of ethyl acetate and heptanes to afford a white solid and the final compound was recrystallised from a mixture of ethyl acetate and heptanes (32% yield).

後処理

  1. filtrationwas filtered through Celite
  2. washwashing with ethanol
  3. concentrationconcentrated in vacuo
  4. customto afford an orange solid
  5. customThis was purified initially
  6. washby eluting on a reverse phase C18 chromatography column (0-60% methanol in water with an acidic modifier) and
  7. concentrationconcentrating the appropriate fractions the crude product
  8. customwas recrystallised from a mixture of ethyl acetate and heptanes
  9. customto afford a white solid

出典と根拠

ORDレコード
ord-1bf6cfd0617e4c169d143c98c50bcda2
出典データセット
uspto-grants-2016_03
特許番号
US09290456B2

反応ノート

読み込み中…