1,3-Dichloropropane → 9-(3-Chloropropyl)-9-cyanofluorene

HRID 850918

反応式

HRID 850918 の反応式
[C:1]([CH:3]1[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)#[N:2].[NH2-].[Na+].[Cl:18][CH2:19][CH2:20][CH2:21]Cl>>[Cl:18][CH2:19][CH2:20][CH2:21][C:3]1([C:1]#[N:2])[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2

参加物

4

実験手順

9-Cyanofluorene was reacted with sodium amide and 1,3-dichloropropane to give 9-(3chloropropyl)-9-cyanofluorene. A solution of 10.0 g. of 9-(3-chloropropyl)-9-cyanofluorene in 200 ml. of morpholine containing 2.0 g. of potassium iodide was stirred at 160° C. for sixteen hours. After cooling the reaction mixture to room temperature, the solution was diluted with 500 ml. of water, and the aqueous mixture was extracted several times with ethylacetate. The organic extracts were combined, washed with water, and the product was extracted therefrom into 0.6 N hydrochloric acid. The aqueous acid layer was separated and made alkaline by the addition of 10 percent sodium hydroxide solution. The alkaline solution was extracted with fresh ethyl acetate, and the extracts were combined, washed with water and dried. Removal of the solvent by evaporation under reduced pressure provided 9-(3-morpholinopropyl)-9-cyanofluorene.

出典と根拠

ORDレコード
ord-f300dec74540491c8781f0e2a07f24a6
出典データセット
uspto-grants-1983_05
特許番号
US04382093

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