反応式
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:14](OC(=O)C)(=[O:16])[CH3:15].[Cl-].[Al+3].[Cl-].[Cl-]>ClC1C=CC=CC=1>[C:14]([C:9]1[CH:8]=[CH:7][C:6]2[C:5]3[C:13](=[CH:1][CH:2]=[CH:3][CH:4]=3)[CH2:12][C:11]=2[CH:10]=1)(=[O:16])[CH3:15]参加物
実験手順
Fluorene is acylated by acetic anhydride in an organic solvent, e.g., chlorobenzene in the presence of aluminum chloride at 18°-20° C at the initial stage of the process followed by heating to 40°-50° C to obtain 2-acetylfluorene at a yield of up to 74 weight percent. The latter is oxidized by chromic acid or by the salts thereof in an acetic acid medium at 50°-90° C for 4-12 hours to obtain 2-acetylfluorenone in a yield of 27-68 weight percent as calculated for 2-acetylfluorene, or 20-50 weight percent when calculated for fluorene. The resultant product is brominated in an organic solvent, e.g., chloroform at 50°-60° C or in acetic acid at 100°-110° C. The yield of the thus-formed 2-ω-dibromoacetylfluorenon equals 71-88 weight percent as calculated for 2-acetylfluorenone, or 35.4-44 weight percent when calculated for fluorene. Then 2-ω-dibromoacetylfluorenone is made to react with morpholine when heated to 50°-98° C for 1-2 hours to obtain 2-ω-bismorpholinoacetylfluorenone in a yield of 40-85 weight percent as calculated for 2-ω-dibromoacetylfluorenone, or 17.6-37.4 weight percent when calculated for fluorene.
後処理
- temperatureby heating to 40°-50° C
出典と根拠
- ORDレコード
- ord-83684ae7b94c42b3a73aaf000530d66e
- 出典データセット
- uspto-grants-1977_04
- 特許番号
- US04016289
関連ノート
読み込み中…