Trifluoroacetic acid → 3,4-Dihydro-2H-1-benzothiopyran-8-amine
반응식
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]2참가 물질
4
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-ad4b85f79fcb43cc906b085571ce6700
- 출처 데이터셋
- uspto-grants-1999_10
- 특허 번호
- US05968954
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