Methanol → Ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate

HRID 236740

반응식

HRID 236740 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]=[C:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1.CO.[BH4-].[Na+]>CC(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][CH:10]1[CH2:11][CH2:12][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:14][CH2:15]1

참가 물질

5

반응물 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 23339072Ethyl 4-[(2,6-dichlorophenyl)imino]-1-piperidinecarboxylate

생성물 1

HCID 23338997Ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a stirred and refluxing mixture of 250 parts of ethyl 4-[(2,6-dichlorophenyl)imino]-1-piperidinecarboxylate in 160 parts of methanol and 160 parts of 2-propanol are added portionwise 30 parts of sodium borohydride. Upon completion, stirring at reflux temperature is continued for one hour. The warm reaction mixture is poured onto water and the product is extracted with methylbenzene. The extract is dried and evaporated. The residue is crystallized from a mixture of 160 parts of 2,2'-oxybispropane and 160 parts of petroleumether, yielding 96 parts of ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate; mp. 107.2°-116.6° C.

후처리

  1. temperaturerefluxing
  2. stirringUpon completion, stirring
  3. temperatureat reflux temperature
  4. customThe warm reaction mixture
  5. additionis poured onto water
  6. extractionthe product is extracted with methylbenzene
  7. customThe extract is dried
  8. customevaporated
  9. customThe residue is crystallized from a mixture of 160 parts of 2,2'-oxybispropane and 160 parts of petroleumether

출처 및 근거

ORD 기록
ord-98d2b936b6444de0bbc2fdcec9ef7811
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04157393

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