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Dimethylamine → 3,6-Bis(dimethylaminoacetyl)-N-ethylcarbazole dihydrochloride dihydrate

HRID 268527
ノート
印刷プレビュー

反応式

HRID 268527 の反応式
[Cl:1][CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:22][CH3:23])[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([C:18](=[O:21])[CH2:19]Cl)=[CH:12][CH:11]=3)=[O:4].C([N:26]1[C:38]2C=CC=CC=2C2[C:27]1=CC=CC=2)C.[Cl:39]CC(Cl)=[O:42].[CH3:44][NH:45][CH3:46].[I-].[K+]>CC(=O)CC>[OH2:4].[OH2:42].[ClH:1].[ClH:39].[CH3:27][N:26]([CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:22][CH3:23])[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([C:18](=[O:21])[CH2:19][N:45]([CH3:46])[CH3:44])=[CH:12][CH:11]=3)=[O:4])[CH3:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 674DimethylamineHCID 4875Potassium IodideHCID 6577Chloroacetyl chlorideHCID 6836N-ethyl carbazoleHCID 215523643,6-bis(chloroacetyl)-N-ethylcarbazole

生成物 1

HCID 215523453,6-Bis(dimethylaminoacetyl)-N-ethylcarbazole dihydrochloride dihydrate

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 14.6 g (0.042 mole) of 3,6-bis(chloroacetyl)-N-ethylcarbazole, prepared from N-ethylcarbazole and chloroacetyl chloride, 100 ml of 40% dimethylamine and 7.0 g of potassium iodide in 200 ml of butanone is placed in a Parr bomb and heated at 70°-80°C with stirring for 2 hours. The reaction mixture is cooled and poured into 2.0 l of ice water. The solid which precipitates is filtered off, dissolved in chloroform and dried over magnesium sulfate to give the free base of the desired product which is subsequently converted to the dihydrochloride salt and recrystallized from methanol-acetone to give the desired product.

後処理

  1. temperatureheated at 70°-80°C
  2. temperatureThe reaction mixture is cooled
  3. customThe solid which precipitates
  4. filtrationis filtered off
  5. dissolutiondissolved in chloroform
  6. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-94345ce1a48443dcae2a0ec1055a67bc
出典データセット
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03947593

反応ノート

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