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

HRID 268527

반응식

HRID 268527 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94345ce1a48443dcae2a0ec1055a67bc
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947593

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