Sodium Hydroxide → 1211518-11-4

HRID 891219노트

반응식

HRID 891219 반응식
[Cl:1]Cl.[NH2:3][C:4]1[N:9]=[C:8](SC)[N:7]=[C:6]([C:12]([F:15])([F:14])[F:13])[N:5]=1.[OH-].[Na+]>C(O)(=O)C>[NH2:3][C:4]1[N:9]=[C:8]([Cl:1])[N:7]=[C:6]([C:12]([F:15])([F:14])[F:13])[N:5]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 22244968HCID 22244968, 화합물

생성물 1

HCID 222449641211518-11-4수율 60%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
20 °C

실험 절차

Chlorine gas was passed into a solution of 21 g of 2-amino-4-methylthio-6-trifluoromethyl-1,3,5-triazine in 0.2 l glacial acetic acid at 20 to 25° C. (15 min). The reaction mixture was stirred for 30 min at approx. 20° C., sprayed for 1 hour with nitrogen gas at room temperature, poured into 1 l of ice-cold aqueous solution of 70 g of sodium hydroxide and stirred for 5 min. After extraction with ethyl acetate, the organic phase was washed with water and dried over magnesium sulfate, and the solvent was removed in vacuo. The crude product was purified by stirring in heptane. After filtration with suction and drying, 12 g (60%) of 2-amino-4-chloro-6-trifluoromethyl-1,3,5-triazine were obtained as a white powder (m.p. 109° C.); 1H NMR (CDCl3): δ=6.4 (s br., 2H).

후처리

  1. custom(15 min)
  2. waitsprayed for 1 hour with nitrogen gas at room temperature
  3. stirringstirred for 5 min
  4. extractionAfter extraction with ethyl acetate
  5. washthe organic phase was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent was removed in vacuo
  8. customThe crude product was purified
  9. stirringby stirring in heptane
  10. filtrationAfter filtration with suction
  11. customdrying

출처 및 근거

ORD 기록
ord-3a9fbc8fc9d94692bfac57c74f3a0eed
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07002011B1

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