Dimethylamine → 3,6-bis(4-dimethylaminobutyryl)-N-ethylcarbazole

HRID 268524

반응식

HRID 268524 반응식
Cl[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[N:11]([CH2:26][CH3:27])[C:12]3[C:17]([C:18]=2[CH:19]=1)=[CH:16][C:15]([C:20](=[O:25])[CH2:21][CH2:22][CH2:23]Cl)=[CH:14][CH:13]=3)=[O:6].C([N:30]1[C:42]2C=CC=CC=2C2[C:31]1=CC=CC=2)C.ClCCCC(Cl)=O.[CH3:50][NH:51][CH3:52].[I-].[K+].[C:55]([OH:62])(=[O:61])/[CH:56]=[CH:57]/[C:58]([OH:60])=[O:59]>O1CCOCC1>[CH3:50][N:51]([CH3:52])[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[N:11]([CH2:26][CH3:27])[C:12]3[C:17]([C:18]=2[CH:19]=1)=[CH:16][C:15]([C:20](=[O:25])[CH2:21][CH2:22][CH2:23][N:30]([CH3:42])[CH3:31])=[CH:14][CH:13]=3)=[O:6].[C:55]([O-:62])(=[O:61])/[CH:56]=[CH:57]/[C:58]([O-:60])=[O:59]

참가 물질

9

반응물 6

HCID 674DimethylamineHCID 4875Potassium IodideHCID 6836N-ethyl carbazoleHCID 783704-Chlorobutyryl chlorideHCID 444972Fumaric AcidHCID 123317903,6-Bis(4-chlorobutyryl)-N-ethylcarbazole

생성물 2

HCID 4613193,6-bis(4-dimethylaminobutyryl)-N-ethylcarbazoleHCID 5460307Fumarate

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 15.8 g (0.039 mole) of 3,6-bis(4-chlorobutyryl)-N-ethylcarbazole, prepared from N-ethylcarbazole and 4-chlorobutyryl chloride, 75 ml of 40% aqueous dimethylamine and 2 g of potassium iodide in 175 ml of p-dioxane is heated in a reaction bomb with stirring for 44 hours. The reaction mixture is concentrated to one-half its original volume in vacuo and diluted with 500 ml of water. The semi-solid which separates is dissolved in ether and washed repeatedly with water and dried over magnesium sulfate to give the free base which is treated with fumaric acid and recrystallized from butanone to give 3,6-bis(4-dimethylaminobutyryl)-N-ethylcarbazole bis acid fumarate. M.P. 94°-98°C.

후처리

  1. temperatureis heated in a reaction bomb
  2. concentrationThe reaction mixture is concentrated to one-half its original volume in vacuo
  3. additiondiluted with 500 ml of water
  4. dissolutionThe semi-solid which separates is dissolved in ether
  5. washwashed repeatedly with water
  6. dry with materialdried over magnesium sulfate
  7. customto give the free base which
  8. customrecrystallized from butanone

출처 및 근거

ORD 기록
ord-98dbf57019ff4ad687fba3e1257f67bf
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947593

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