Desipramine Hydrochloride → HCID 14750714、化合物

HRID 621697

反応式

HRID 621697 の反応式
Cl.[C:2](Cl)(=[O:9])[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1.C(=O)(O)[O-].[Na+].[CH3:16][NH:17][CH2:18][CH2:19][CH2:20][N:21]1[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[CH2:29][CH2:28][C:27]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]1=2.Cl>C(Cl)Cl>[CH3:16][N:17]([C:2]([C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1)=[O:9])[CH2:18][CH2:19][CH2:20][N:21]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:27]=2[CH2:28][CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]1=2

参加物

5

反応物 3

HCID 65327Desipramine HydrochlorideHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 516892Sodium Bicarbonate

生成物 1

HCID 14750714HCID 14750714、化合物収率 62%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
5 °C

実験手順

Freshly prepared nicotinoyl chloride hydrochloride (0.55 g, 0.003 mol) was suspended in methylene chloride (12 ml) cooled to 5° C. and sodium bicarbonate (0.053 g, 0.0063 mol) was added. After 5 minutes, desipramine hydrochloride (0.75 g, 0.0025 mol) was added and the mixture was stirred for 3 hours at 5° C. The sodium chloride was removed by filtration and the organic solution was extracted with aqueous sodium bicarbonate, dried over sodium sulfate, filtered through Celite™ and concentrated. Ethyl ether (5 ml) was added to the oily residue and white crystals formed. Yield 62% (0.58 g), m.p. 84°-86° C. The product has the formula: ##STR1616##

後処理

  1. customThe sodium chloride was removed by filtration
  2. extractionthe organic solution was extracted with aqueous sodium bicarbonate
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered through Celite™
  5. concentrationconcentrated
  6. additionEthyl ether (5 ml) was added to the oily residue and white crystals
  7. customformed

出典と根拠

ORDレコード
ord-17821f5355284f8e935f4fa6162d6dfb
出典データセット
uspto-grants-1989_04
特許番号
US04824850

関連ノート

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