Diboron → 3-Hydroxymethyl-10,11-dihydrodibenzo[b,f]thiepin
反応式
[CH:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[S:6][C:5]=2[CH:4]=[C:3]([C:16](O)=[O:17])[CH:2]=1.B#B>O1CCCC1.O>[OH:17][CH2:16][C:3]1[CH:2]=[CH:1][C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[S:6][C:5]=2[CH:4]=1参加物
5
実験手順
Dissolve 7.5 gm. of 10,11-dihydrodibenzo[b,f]-thiepin-3-carboxylic acid in 140 ml. of tetrahydrofuran. With stirring, add 90 ml. of 1 N diborane in tetrahydrofuran. Stir at room temperature for 2 hours and dilute the reaction mixture with water. Extract into ether, and evaporate the ether extract to dryness. Stir the residue with hexane and filter to obtain the title product (m.p., 82°-84° C.).
後処理
- dissolutionDissolve 7.5 gm
- additionadd 90 ml
- stirringStir at room temperature for 2 hours
- extractionExtract into ether
- customevaporate the ether
- extractionextract to dryness
- stirringStir the residue with hexane
- filtrationfilter
出典と根拠
- ORDレコード
- ord-b0b2b82bec164028997e437c011ae2bf
- 出典データセット
- uspto-grants-1980_12
- 特許番号
- US04237160
反応ノート
読み込み中…