Triethylamine → HCID 22909583、化合物

HRID 1379060ノート

反応式

HRID 1379060 の反応式
[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:8][CH:9]2[CH2:14][CH2:13][CH2:12][CH2:11][NH:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[CH3:28][O:29][C:30]1[CH:31]=[C:32]([CH2:38][C:39](Cl)=[O:40])[CH:33]=[CH:34][C:35]=1[O:36][CH3:37]>C(Cl)Cl>[CH3:28][O:29][C:30]1[CH:31]=[C:32]([CH2:38][C:39]([N:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH:9]2[CH2:8][CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:40])[CH:33]=[CH:34][C:35]=1[O:36][CH3:37]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 3604458(3,4-Dimethoxyphenyl)acetyl chlorideHCID 4544491HCID 4544491、化合物

生成物 1

HCID 22909583HCID 22909583、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 2.65 g (0.01M) of 2-(2,2-diphenylethyl)piperidine in 25 ml of methylene chloride containing 1.5 ml of triethylamine was cooled in ice and a solution of 2.35 g (0.011M) of 3,4-di-methoxyphenylacetyl chloride in 25 ml of methylene chloride was added dropwise. The cooling bath was removed and the mixture was stirred at room temperature overnight. The mixture was then washed with dilute hydrochloric acid, water, dilute sodium hydroxide and saturated sodium chloride solution. Removal of the solvent left an oil which was purified by chromatography on silica gel. The solid thus obtained melted at 113°-114° C. after recrystallization from cyclohexane-ethyl acetate.

後処理

  1. customThe cooling bath was removed
  2. washThe mixture was then washed with dilute hydrochloric acid, water, dilute sodium hydroxide and saturated sodium chloride solution
  3. customRemoval of the solvent
  4. waitleft an oil which
  5. customwas purified by chromatography on silica gel
  6. customThe solid thus obtained melted at 113°-114° C. after recrystallization from cyclohexane-ethyl acetate

出典と根拠

ORDレコード
ord-857268e8d3c74371b1560fecf6b4f08d
出典データセット
uspto-grants-1997_09
特許番号
US05670521

反応ノート

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