Sulfuric Acid → Ethyl 3-(benzyloxy)-4-oxopiperidine-1-carboxylate

HRID 1088352ノート

反応式

HRID 1088352 の反応式
C[O:2][C:3]1(OC)[CH2:8][CH2:7][N:6]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:5][CH:4]1[O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.S(=O)(=O)(O)O>O>[O:2]=[C:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:5][CH:4]1[O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 3019743Ethyl 4,4-dimethoxy-3-(phenylmethoxy)piperidine-1-carboxylate

生成物 1

HCID 3019711Ethyl 3-(benzyloxy)-4-oxopiperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 94 parts of ethyl 4,4-dimethoxy-3-(phenylmethoxy)-1-piperidinecarboxylate and 2300 parts of a sulfuric acid solution 1% in water was stirred and refluxed for 2.50 hours. The reaction mixture was cooled and the product was extracted three times with dichloromethane. The combined extracts were washed with a small amount of water, dried, filtered and evaporated. The residue was taken up in methylbenzene and the latter was evaporated again. The residue was stirred in petroleum ether. The latter was separated and the solvent was evaporated, yielding 64.9 parts of ethyl 4-oxo-3-(phenylmethoxy)-1-piperidinecarboxylate as a residue (intermediate 50).

後処理

  1. temperaturerefluxed for 2.50 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionthe product was extracted three times with dichloromethane
  4. washThe combined extracts were washed with a small amount of water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customthe latter was evaporated again
  9. stirringThe residue was stirred in petroleum ether
  10. customThe latter was separated
  11. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-d4c82bf49a374db8acca0e07991709fc
出典データセット
uspto-grants-1990_10
特許番号
US04962115

反応ノート

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