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Phenylacetyl chloride → Ethyl 4-[(4-chlorophenyl)(phenylacetyl)amino]piperidine-1-carboxylate

HRID 26740
ノート
印刷プレビュー

反応式

HRID 26740 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[C:20]1([CH2:26][C:27](Cl)=[O:28])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:13][CH2:14]2)[C:27](=[O:28])[CH2:26][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7679Phenylacetyl chlorideHCID 2846949Ethyl 4-[(4-chlorophenyl)amino]piperidine-1-carboxylate

生成物 1

HCID 3017393Ethyl 4-[(4-chlorophenyl)(phenylacetyl)amino]piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a stirred solution of 58 parts of ethyl 4-[(4-chlorophenyl)amino]-1-piperidinecarboxylate in 240 parts of benzene is added dropwise a solution of 46.2 parts of benzeneacetyl chloride in 80 parts of benzene at a temperature between 40°-70° C. Upon completion, the whole is stirred and refluxed for 6h.15. The reaction mixture is cooled and filtered. The filtrate is washed successively with water, sodium hydrogen carbonate solution and water, then dried and evaporated in vacuo. The residue is crystallized from 1,1'-oxybisethane, yielding 47 parts of ethyl 4-[N-(4-chlorophenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 108° C.

後処理

  1. temperaturerefluxed for 6h.15
  2. temperatureThe reaction mixture is cooled
  3. filtrationfiltered
  4. washThe filtrate is washed successively with water, sodium hydrogen carbonate solution and water
  5. customdried
  6. customevaporated in vacuo
  7. customThe residue is crystallized from 1,1'-oxybisethane

出典と根拠

ORDレコード
ord-8aaa4720a16b49f8bea42b285509376e
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04151286

反応ノート

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