Trifluoroacetic acid → HCID 12873978、化合物

HRID 443899ノート

反応式

HRID 443899 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

反応物 3

HCID 6422Trifluoroacetic acidHCID 6586872,3-Dihydroimidazo(2,1-b)benzothiazol-6-amineHCID 4311764Sodium borohydride

生成物 1

HCID 12873978HCID 12873978、化合物

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-4ab475c3118f4cb98f077b31627c48ee
出典データセット
uspto-grants-1981_04
特許番号
US04262004

反応ノート

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