O-ethyl 1-(phenylmethyl)-4-piperidineethanimidate hydrochloride → HCID 14012850、化合物

HRID 2309618ノート

反応式

HRID 2309618 の反応式
Cl.[C:2]1([CH2:8][N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][C:16](=[NH:20])OCC)[CH2:11][CH2:10]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:21][C:22]1[CH:27]=[CH:26][C:25]([CH2:28][NH:29][C:30]2[C:31](N)=[CH:32][CH:33]=[CH:34][CH:35]=2)=[CH:24][CH:23]=1>CO>[CH3:21][C:22]1[CH:23]=[CH:24][C:25]([CH2:28][N:29]2[C:30]3[CH:31]=[CH:32][CH:33]=[CH:34][C:35]=3[N:20]=[C:16]2[CH2:15][CH:12]2[CH2:11][CH2:10][N:9]([CH2:8][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:14][CH2:13]2)=[CH:26][CH:27]=1

参加物

4

反応物 2

HCID 14518093O-ethyl 1-(phenylmethyl)-4-piperidineethanimidate hydrochloride2 回HCID 14518103HCID 14518103、化合物

生成物 1

HCID 14012850HCID 14012850、化合物収率 63%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 116.5 parts of O-ethyl 1-(phenylmethyl)-4-piperidineethanimidate hydrochloride, 61.5 parts of N1 -[(4-methylphenyl)methyl]-1,2-benzenediamine and 400 parts of methanol was stirred and refluxed overnight. Another portion of 40 parts of O-ethyl 1-(phenylmethyl)-4-piperidineethanimidate hydrochloride was added and stirring was continued for 4 hours at reflux. The reaction mixture was evaporated. Water was added to the residue. The solution was treated with ammonium hydroxide. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 74.5 parts (63%) of 1-[(4-methylphenyl)methyl]-2-[[1-(phenylmethyl)-4-piperidinyl]methyl]-1H-benzimidazole; mp. 124.2° C. (6).

後処理

  1. temperaturerefluxed overnight
  2. stirringstirring
  3. temperatureat reflux
  4. customThe reaction mixture was evaporated
  5. additionWater was added to the residue
  6. additionThe solution was treated with ammonium hydroxide
  7. extractionThe product was extracted with trichloromethane
  8. customThe extract was dried
  9. filtrationfiltered
  10. customevaporated
  11. customThe residue was crystallized from acetonitrile
  12. filtrationThe product was filtered off
  13. customdried

出典と根拠

ORDレコード
ord-a8ba8855c88441898f26ca14a030173e
出典データセット
uspto-grants-1987_09
特許番号
US04695575

反応ノート

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