Ethyl chloroformate → Ethyl 3-methyl-4-oxopiperidine-1-carboxylate

HRID 466540

反応式

HRID 466540 の反応式
[CH3:1][CH:2]1[C:7](=[O:8])[CH2:6][CH2:5][N:4](CC2C=CC=CC=2)[CH2:3]1.[C:16](Cl)(=[O:20])[O:17][CH2:18][CH3:19]>CC1C=CC=CC=1>[CH3:1][CH:2]1[C:7](=[O:8])[CH2:6][CH2:5][N:4]([C:16]([O:17][CH2:18][CH3:19])=[O:20])[CH2:3]1

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 5609651-Benzyl-3-methyl-4-piperidone

生成物 1

HCID 15075657Ethyl 3-methyl-4-oxopiperidine-1-carboxylate収率 83%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred solution of 152 parts of 3-methyl-1-(phenylmethyl)-4-piperidinone in 900 parts of methylbenzene were added dropwise 218 parts of ethyl carbonochloridate at room temperature. Upon completion, stirring was continued overnight at reflux. After cooling, the reaction mixture was washed with water and hydrochloric acid, dried, filtered and evaporated. The residue was distilled, yielding 120.5 parts (83%) of ethyl 3-methyl-4-oxo-1-piperidinecarboxylate; bp. 98°-105° C. at 1 mm pressure (intermediate 26).

後処理

  1. temperatureat reflux
  2. temperatureAfter cooling
  3. washthe reaction mixture was washed with water and hydrochloric acid
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-13d868faa37847a28507459d1e747ed7
出典データセット
uspto-grants-1992_10
特許番号
US05157035

関連ノート

読み込み中…