Nitrogen → 6966-30-9

HRID 1109837노트

반응식

HRID 1109837 반응식
C([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9](=[O:16])[C:10](=[N:14]O)[C:11]([OH:13])=[O:12])C.N(=C1C=CC=C[CH:20]1[C:21](CC(OCC)=O)=[O:22])O.[C:33](OC(=O)C)(=O)[CH3:34].[H][H].N#N>[Pd].C(O)(=O)C>[C:21]([NH:14][CH:10]([C:9](=[O:16])[C:4]1[CH:3]=[CH:8][CH:7]=[CH:6][CH:5]=1)[C:11]([O:13][CH2:33][CH3:34])=[O:12])(=[O:22])[CH3:20]

참가 물질

7

반응물 4

HCID 947NitrogenHCID 7918Acetic AnhydrideHCID 178418361HCID 178418361, 화합물HCID 178472165HCID 178472165, 화합물

생성물 1

HCID 2272876966-30-9수율 209.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

With stirring, a mixture of 221 g of ethyl 2-oximinobenzoylacetate (ethyl 2-oximino-3-oxo-3-phenylpropionate), 500 g of acetic anhydride, 50 g of glacial acetic acid and 20 g of a Pd/C catalyst (EF 101 R/W 51% H2O, sold by Degussa) is hydrogenated under normal pressure at 60° C. over 4 hours. The hydrogen uptake is 40 l. Afterwards the reactor is made inert with N2, flushed with nitrogen and the catalyst is removed by filtration. The filtrate is subsequently concentrated under reduced pressure on a rotary evaporator to give a residue (259.3 g), which is recrystallised from 200 ml of isopropanol/500 ml of petroleum ether.

후처리

  1. customflushed with nitrogen
  2. customthe catalyst is removed by filtration
  3. concentrationThe filtrate is subsequently concentrated under reduced pressure on a rotary evaporator

출처 및 근거

ORD 기록
ord-e892b295ae4e4c9cb1ea0185f90691bf
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322964

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