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Benzoyl chloride → N-(4-benzyl-4-dimethylaminocyclohexyl)-N-propylbenzamide hydrochloride

HRID 1179038
ノート
印刷プレビュー

反応式

HRID 1179038 の反応式
[CH3:1][N:2]([CH3:19])[C:3]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:8][CH2:7][CH:6]([NH:9][CH2:10][CH2:11][CH3:12])[CH2:5][CH2:4]1.[CH2:20](N(CC)CC)C.[C:27]([Cl:35])(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[OH-].[K+]>C(Cl)Cl.CN(C1C=CN=CC=1)C.O>[ClH:35].[CH2:13]([C:3]1([N:2]([CH3:1])[CH3:19])[CH2:4][CH2:5][CH:6]([N:9]([CH2:10][CH2:11][CH3:12])[C:27](=[O:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:7][CH2:8]1)[C:18]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 14797Potassium HydroxideHCID 9856507N,N-dimethyl-1-phenyl-N'-propyl-cyclohexane-1,4-diamine

生成物 1

HCID 69338285N-(4-benzyl-4-dimethylaminocyclohexyl)-N-propylbenzamide hydrochloride

試薬・触媒・溶媒 3

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

1.00 g of the polar diastereomer of N,N-dimethyl-1-phenyl-N′-propyl-cyclohexane-1,4-diamine (see example 6) were dissolved in 15 ml methylene chloride, and 560 μl triethylamine and approx. 10 mg DMAP were added. 468 μl benzoyl chloride were added dropwise, while cooling in an ice/methanol bath, and the reaction mixture was then stirred overnight, while warming to room temperature. For working up, 12 ml five molar KOH solution and 12 ml water were added, the mixture was stirred for ten minutes and extracted three times with 25 ml methylene chloride each time, the combined extracts were dried over magnesium sulfate and filtered and the filtrate was concentrated. From the product obtained (1.29 g), 752 mg of the polar diastereomer of N-(4-benzyl-4-dimethylamino-cyclohexyl)-N-propyl-benzamide hydrochloride were prepared as described for example 1 with water and chlorotrimethylsilane in 2-butanone.

後処理

  1. temperaturewhile cooling in an ice/methanol bath
  2. stirringthe mixture was stirred for ten minutes
  3. extractionextracted three times with 25 ml methylene chloride each time
  4. dry with materialthe combined extracts were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-bb32193a2e6440fd885afaa30d7b64ee
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07276518B2

反応ノート

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