Sodium Hydroxide → HCID 12040787, 화합물

HRID 891218노트

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HRID 891218 반응식
[Cl:1]Cl.[NH2:3][C:4]1[N:9]=[C:8](SC)[N:7]=[C:6]([CH:12]([F:14])[CH3:13])[N:5]=1.[OH-].[Na+]>C(O)(=O)C>[NH2:3][C:4]1[N:9]=[C:8]([Cl:1])[N:7]=[C:6]([CH:12]([F:14])[CH3:13])[N:5]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 222449654-(1-Fluoroethyl)-6-(methylthio)-1,3,5-triazin-2-amine

생성물 1

HCID 12040787HCID 12040787, 화합물수율 70%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
20 °C

실험 절차

Chlorine gas was passed into a suspension of 38 g of 2-amino-4-methylthio-6-(1-fluoroethyl)-1,3,5-triazine in 0.25 l of glacial acetic acid (15 min) at 20 to 25° C. The reaction mixture was stirred for 30 min at approx. 20° C., sprayed for 1 hour with nitrogen gas at room temperature, poured into 1.25 l of ice-cold aqueous solution of 87 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, 25 g (70%) of 2-amino-4-chloro-6-(1-fluoroethyl)-1,3,5-triazine were obtained as a white powder (m.p. 131° C.); 1H NMR (CDCl3): δ=1.7 (dd, 3 H), 5.4 (dq, 1 H), 6.1 (s br., 1 H), 6.7 (s br., 1H).

후처리

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

출처 및 근거

ORD 기록
ord-723b383e40c342508da3f2f11da2cb75
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07002011B1

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