11-Methylene-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic acid → 11-Methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid
反応式
[CH2:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2>[Pd].C(O)C>[CH3:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2参加物
4
実験手順
Dissolve 514 mg of 11-methylene-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic acid in 150 ml. of ethanol. Add 100 mg of 5% palladium on carbon catalyst. Hydrogenate at 20 psi for 30 minutes. Filter and strip the filtrate to dryness. Recrystallize the residue from isopropanol to obtain the title product (yield 365 mg, m.p. 224°-226° C.).
後処理
- filtrationFilter
- customRecrystallize the residue from isopropanol
出典と根拠
- ORDレコード
- ord-5c4ef8f90bd149b48d2a71d8c3ea4744
- 出典データセット
- uspto-grants-1981_08
- 特許番号
- US04282365
反応ノート
読み込み中…