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

HRID 26736

反応式

HRID 26736 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0fc4a7895f4a4ca7afdf6601906011b4
出典データセット
uspto-grants-1979_04
特許番号
US04151286

関連ノート

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