HCID 86677027, 화합물 → HCID 178435906, 화합물

HRID 927174노트

반응식

HRID 927174 반응식
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

참가 물질

4

반응물 2

HCID 86677027HCID 86677027, 화합물2회HCID 1785188083-Hydroxy-6-(2-Phenylethyl)pyridazin-4(1h)-One

생성물 1

HCID 178435906HCID 178435906, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1bf6cfd0617e4c169d143c98c50bcda2
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290456B2

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