Piperidine → 1-[4-(15-Carbomethoxypentadecylamino)benzoyl]piperidine

HRID 904260ノート

反応式

HRID 904260 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.CN(C1C=CC=CN=1)C.Cl.[C:24]([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][NH:43][C:44]1[CH:52]=[CH:51][C:47]([C:48](Cl)=[O:49])=[CH:46][CH:45]=1)([O:26][CH3:27])=[O:25]>CCOCC>[C:24]([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][NH:43][C:44]1[CH:52]=[CH:51][C:47]([C:48]([N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[O:49])=[CH:46][CH:45]=1)([O:26][CH3:27])=[O:25]

参加物

6

反応物 4

HCID 8082PiperidineHCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 211632694-(15-Carbomethoxypentadecylamino)benzoyl chloride hydrochloride

生成物 1

HCID 211633521-[4-(15-Carbomethoxypentadecylamino)benzoyl]piperidine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a chilled solution of 35 ml. of piperidine, 2.5 ml. of triethylamine and 0.6 g. of dimethylaminopyridine in 100 ml. of diethyl ether is added (1/2 hour) a solution of 8.3 g. of 4-(15-carbomethoxypentadecylamino)benzoyl chloride hydrochloride in 50 ml. of ether. The solution is warmed to room temperature and maintained there for two hours. The solution is heated to reflux for an additional 2 hours at which time the reaction is complete. The solution is cooled, extracted twice with 100 ml. portions of water and dried over magnesium sulfate. The solvent is removed in vacuo and the solid is recrystallized in 50 ml. of diethyl ether to yield the product.

後処理

  1. temperaturemaintained there for two hours
  2. temperatureThe solution is heated
  3. temperatureto reflux for an additional 2 hours at which time the reaction
  4. temperatureThe solution is cooled
  5. extractionextracted twice with 100 ml
  6. dry with materialportions of water and dried over magnesium sulfate
  7. customThe solvent is removed in vacuo
  8. customthe solid is recrystallized in 50 ml
  9. customof diethyl ether to yield the product

出典と根拠

ORDレコード
ord-0cf26cd075654c1dbc3850254e4f5b92
出典データセット
uspto-grants-1980_10
特許番号
US04230628

反応ノート

読み込み中…