Trifluoroacetic acid → HCID 12873978、化合物

HRID 1759405ノート

反応式

HRID 1759405 の反応式
[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]=1

参加物

4

実験手順

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.

後処理

  1. filtrationThe precipitated product is filtered off
  2. washwashed with water
  3. washThe mixture is washed with ammonium hydroxide
  4. customThe organic phase is dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is crystallized from acetonitrile

出典と根拠

ORDレコード
ord-bdaf1945ea5445edba57808a53775307
出典データセット
uspto-grants-1982_07
特許番号
US04340738

反応ノート

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