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

HRID 486436

반응식

HRID 486436 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 15075657Ethyl 3-methyl-4-oxopiperidine-1-carboxylate수율 83%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-abcf0f1d31534ab2b8f0fd36767139f3
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292738

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