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

HRID 3922

반응식

HRID 3922 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-17f6266b5d2e48cc810a4fc82883f5f9
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723010

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