Ethanol → N-(6-Methylhept-5-en-3-ylidene)hydroxylamine

HRID 1165086ノート

反応式

HRID 1165086 の反応式
[C:1]1(P(C2C=CC=CC=2)C2C=CC=CC=2)[CH:6]=CC=C[CH:2]=1.C(O)=O.C([N:25]([CH2:28][CH3:29])CC)C.[OH2:30].[CH2:31](Cl)Cl.[CH2:34](O)[CH3:35]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:2][C:1](=[CH:34][CH2:35][C:28](=[N:25][OH:30])[CH2:29][CH3:31])[CH3:6]

参加物

7

反応物 5

HCID 702Ethanol2 回HCID 962WaterHCID 6344DichloromethaneHCID 11776TriphenylphosphineHCID 11084032Triethylammonium formate

生成物 1

HCID 71334023N-(6-Methylhept-5-en-3-ylidene)hydroxylamine

試薬・触媒・溶媒 1

HCID 167845palladium(II) acetate触媒

実験手順

An aliquot (0.5 mole) of the resultinge compound was reacted under stirring for 1 hour together with 0.005 mole of palladium acetate, 0.02 mole of tripenylphosphine, 1.5 moles of triethylamine formate, 20 moles of ethanol and 12 moles of water. After the reaction, ethanol was evaporated from the reaction mixture under reduced pressure. Ten moles of methylene chloride was added to the residue, and the mixture was washed with water. The solvent was evaporated, and the residue was purified by silica gel column chromatography to give 2-methyl-5-hydroxyimino-2-heptene in a yield of 96 mole %. A quantitative analysis of the reaction mixture by gas chromatography showed that the reaction proceeded quantitatively.

後処理

  1. customwas evaporated from the reaction mixture under reduced pressure
  2. washthe mixture was washed with water
  3. customThe solvent was evaporated
  4. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-920fba8d918a4666a4d5ed7354e03fca
出典データセット
uspto-grants-1990_03
特許番号
US04906768

反応ノート

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