Nitrogen → 6966-30-9

HRID 1109837ノート

反応式

HRID 1109837 の反応式
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]

参加物

7

反応物 4

HCID 947NitrogenHCID 7918Acetic AnhydrideHCID 178418361HCID 178418361、化合物HCID 178472165HCID 178472165、化合物

生成物 1

HCID 2272876966-30-9収率 209.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e892b295ae4e4c9cb1ea0185f90691bf
出典データセット
uspto-grants-1994_06
特許番号
US05322964

反応ノート

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