2-Chloro-1,1,1-triethoxyethane → 2-(Chloromethyl)-5-(trifluoromethyl)-1,3-benzothiazole

HRID 3922

反応式

HRID 3922 の反応式
Cl.[NH2:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[CH:5][C:4]=1[SH:13].[Cl:14][CH2:15][C:16](OCC)(OCC)OCC>C(O)C>[Cl:14][CH2:15][C:16]1[S:13][C:4]2[CH:5]=[CH:6][C:7]([C:9]([F:10])([F:11])[F:12])=[CH:8][C:3]=2[N:2]=1

参加物

4

反応物 2

HCID 3059222-Chloro-1,1,1-triethoxyethaneHCID 27346782-Amino-4-(trifluoromethyl)benzenethiol hydrochloride

生成物 1

HCID 142042052-(Chloromethyl)-5-(trifluoromethyl)-1,3-benzothiazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of 2-amino-4-trifluoromethylthiophenol hydrochloride (30.0 g) in ethanol (125 ml) was added 2-chloro-1,1,1-triethoxyethane (31.0 g). The mixture was heated for 1 hour at 60° C. The solution was concentrated to remove excess ethanol and the resulting material was extracted with ether (500 ml). The organic extract was washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml), and then evaporated to obtain an amber colored oil, which crystallized upon standing at room temperature (28.9 g; m.p. 52° C).

後処理

  1. concentrationThe solution was concentrated
  2. customto remove excess ethanol
  3. extractionthe resulting material was extracted with ether (500 ml)
  4. extractionThe organic extract
  5. washwas washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml)
  6. customevaporated
  7. customto obtain an amber colored oil, which
  8. customcrystallized
  9. customupon standing at room temperature

出典と根拠

ORDレコード
ord-17f6266b5d2e48cc810a4fc82883f5f9
出典データセット
uspto-grants-1988_02
特許番号
US04723010

関連ノート

読み込み中…