Acetic Acid → Methyl [4-(aminomethyl)phenoxy]acetate acetate

HRID 733511노트

반응식

HRID 733511 반응식
O[N:2]=[CH:3][C:4]1[CH:15]=[CH:14][C:7]([O:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:6][CH:5]=1.C(O)(=O)C.N#N>CO.[Pd]>[C:10]([OH:12])(=[O:11])[CH3:9].[NH2:2][CH2:3][C:4]1[CH:15]=[CH:14][C:7]([O:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 947NitrogenHCID 73461790Methyl {4-[(hydroxyimino)methyl]phenoxy}acetate

생성물 1

HCID 86028338Methyl [4-(aminomethyl)phenoxy]acetate acetate수율 162.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of methyl {4-[(hydroxyimino)methyl]phenoxy}acetate (30 g, 0.14 mol) in methanol (650 mL) was added glacial acetic acid (6.8 g) and passed N2 for 30 min. To this was added Pd/C (10%, 3 g) and hydrogenated under 2 bars of pressure for 12 h. The reaction mixture was concentrated under vacuum. The crude product was treated with EtOAc (500 mL) and the white product filtered off The solid was dried under vacuum to give the title compound (29 g, 81%).

후처리

  1. customfor 30 min
  2. concentrationThe reaction mixture was concentrated under vacuum
  3. additionThe crude product was treated with EtOAc (500 mL)
  4. filtrationthe white product filtered off The solid
  5. customwas dried under vacuum

출처 및 근거

ORD 기록
ord-fb2be3a7a0ff46b7897414ab1a99b24c
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589232B2

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