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

HRID 1165086노트

반응식

HRID 1165086 반응식
[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]

참가 물질

7

반응물 5

HCID 702Ethanol2회HCID 962WaterHCID 6344DichloromethaneHCID 11776TriphenylphosphineHCID 11084032Triethylammonium formate

생성물 1

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

시약·촉매·용매 1

HCID 167845palladium(II) acetate촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-920fba8d918a4666a4d5ed7354e03fca
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906768

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