Hydrochloric Acid → Ethyl 2-methyl-2-(piperidin-4-YL)propanoate

HRID 977161ノート

反応式

HRID 977161 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:22])[C:6]([CH3:21])([CH3:20])[C:7]1[CH2:8][CH2:9][N:10](CC2C=CC=CC=2)[CH2:11][CH:12]=1)[CH3:3].[H][H].[OH-].[Na+]>C(O)C.O.[Pd]>[CH2:2]([O:4][C:5](=[O:22])[C:6]([CH3:21])([CH3:20])[CH:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1)[CH3:3]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 545483681-Phenylmethyl-alpha,alpha-dimethyl-1,2,3,6-tetrahydro-4-pyridine-acetic acid ethyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 49759624Ethyl 2-methyl-2-(piperidin-4-YL)propanoate収率 82%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 246 g (76.6×10-2 mole) of the hydrochloride of 1-phenylmethyl-α,α-dimethyl-1,2,3,6-tetrahydro-4-pyridine-acetic acid ethyl ester in 1.5 liters of ethanol was hydrogenated in a Parr's apparatus at 50° C. at a hydrogen pressure of 3.106Pa in the presence of 20 g of 5% palladium/charcoal. After filtering, the filtrate obtained was evaporated off under reduced pressure. The residue obtained was taken up in water and rendered alkaline with 500 ml of 5N sodium hydroxide. It was extracted with ethyl acetate. The organic phase was dried over magnesium sulphate and filtered and the solvents were evaporated off under reduced pressure. 125.3 g (yield: 82%) of the desired product was obtained as an oil. n21 =1.47

後処理

  1. filtrationAfter filtering
  2. customthe filtrate obtained
  3. customwas evaporated off under reduced pressure
  4. customThe residue obtained
  5. extractionIt was extracted with ethyl acetate
  6. dry with materialThe organic phase was dried over magnesium sulphate
  7. filtrationfiltered
  8. customthe solvents were evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-073a01532a0944e0b1b5c8cc5092b470
出典データセット
uspto-grants-1997_03
特許番号
US05614534

反応ノート

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