Trifluoroacetic acid → HCID 12873978, 화합물
반응식
[F:1][C:2]([F:7])([F:6])[C:3](O)=O.[BH4-].[Na+].[N:10]1[CH2:11][CH2:12][N:13]2[C:17]3[CH:18]=[C:19]([NH2:22])[CH:20]=[CH:21][C:16]=3[S:15][C:14]=12>>[F:1][C:2]([F:7])([F:6])[CH2:3][NH:22][C:19]1[CH:20]=[CH:21][C:16]2[S:15][C:14]3=[N:10][CH2:11][CH2:12][N:13]3[C:17]=2[CH:18]=1참가 물질
4
실험 절차
To a stirred mixture of 60 parts of trifluoroacetic acid and 4 parts of sodium borohydride are added portionwise, during a 5 hours-period, 4 parts of 2,3-dihydroimidazo[2,1-b]benzothiazol-6-amine at 30°-40° C. The reaction mixture is poured onto 300 parts of ice-water. The precipitated product is filtered off, washed with water and taken up in trichloromethane. The mixture is washed with ammonium hydroxide. The organic phase is dried, filtered and evaporated. The residue is crystallized from acetonitrile, yielding 3.3 parts of 2,3-dihydro-N-(2,2,2-trifluoroethyl)imidazo[2,1-b]benzothiazol-6-amine; mp. 211.7° C.
후처리
- filtrationThe precipitated product is filtered off
- washwashed with water
- washThe mixture is washed with ammonium hydroxide
- customThe organic phase is dried
- filtrationfiltered
- customevaporated
- customThe residue is crystallized from acetonitrile
출처 및 근거
- ORD 기록
- ord-4ab475c3118f4cb98f077b31627c48ee
- 출처 데이터셋
- uspto-grants-1981_04
- 특허 번호
- US04262004
반응 노트
불러오는 중…