Trifluoroacetic acid → 3,4-Dihydro-2H-1-benzothiopyran-8-amine
反応式
C(OC([NH:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[S:17][CH2:16][CH2:15][CH2:14]2)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[S:17][CH2:16][CH2:15][CH2:14]2参加物
4
実験手順
10 g (37.7 mmol) of the compound obtained in Step 1 above in 50 ml of dichloromethane are mixed with 50 ml of trifluoroacetic acid, and the mixture is stirred for 30 minutes at room temperature and then evaporated to dryness. The residue is taken up in ether and the solid obtained is filtered off and treated with N sodium hydroxide solution. The aqueous phase is extracted with ether and the ethereal phases are combined, dried over magnesium sulphate and concentrated to yield 4.48 g of the desired product (theory: 6.2 g).
後処理
- customevaporated to dryness
- customthe solid obtained
- filtrationis filtered off
- additiontreated with N sodium hydroxide solution
- extractionThe aqueous phase is extracted with ether
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-ad4b85f79fcb43cc906b085571ce6700
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05968954
反応ノート
読み込み中…