Dimethylamine → HCID 21552345、化合物

HRID 268527

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

7

反応物 5

HCID 674DimethylamineHCID 4875Potassium IodideHCID 6577Chloroacetyl chlorideHCID 6836N-ethyl carbazoleHCID 21552364HCID 21552364、化合物

生成物 1

HCID 21552345HCID 21552345、化合物

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
特許番号
US03947593

関連ノート

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