Dimethylformamide → N-(4-tert-pentylbenzyl)-N-methyl-1-naphthylmethylamine hydrochloride

HRID 1493376

反応式

HRID 1493376 の反応式
[CH3:1][NH:2][CH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1.C(=O)([O-])[O-].[Na+].[Na+].CN(C)C=O.[C:25]([C:30]1[CH:37]=[CH:36][C:33]([CH2:34][Cl:35])=[CH:32][CH:31]=1)([CH2:28][CH3:29])([CH3:27])[CH3:26]>O>[ClH:35].[C:25]([C:30]1[CH:37]=[CH:36][C:33]([CH2:34][N:2]([CH2:3][C:4]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH:7]=[CH:6][CH:5]=2)[CH3:1])=[CH:32][CH:31]=1)([CH2:28][CH3:29])([CH3:27])[CH3:26]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 84474N-Methyl-N-naphthylmethylamineHCID 141400Toluene, alpha-chloro-p-(1,1-dimethyl-propyl)-

生成物 1

HCID 18957493N-(4-tert-pentylbenzyl)-N-methyl-1-naphthylmethylamine hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 1.03 g of N-methyl-1-naphthylmethylamine, 0.7 g of sodium carbonate and 10 ml of dimethylformamide was added 1.3 g of 4-tert-pentylbenzyl chloride and was stirred at room temperature for 16 hours. The reaction mixture was poured into water and extracted with benzene, and the benzene solution was washed with water. After distilling away benzene, 1.5 ml of concentrated hydrochloric acid was added and then an excess of concentrated hydrochloric acid was removed. A small amount of acetone was added and 1.33 g of formed white crystal was filtrated. White crystal of N-(4-tert-pentylbenzyl)-N-methyl-1-naphthylmethylamine hydrochloride (Compound of Example 12) was obtained by recrystallization from acetone.

後処理

  1. extractionextracted with benzene
  2. washthe benzene solution was washed with water
  3. distillationAfter distilling away benzene, 1.5 ml of concentrated hydrochloric acid
  4. additionwas added
  5. customan excess of concentrated hydrochloric acid was removed
  6. additionA small amount of acetone was added
  7. filtration1.33 g of formed white crystal was filtrated

出典と根拠

ORDレコード
ord-82620228dad3454db0761321bfbaee7c
出典データセット
uspto-grants-1991_06
特許番号
US05021458

関連ノート

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