1-Bromo-4-fluorobutane → 7-Chloro-4-(4-fluorobutyl)-4H-1,2,4-benzothiadiazine 1,1-dioxide

HRID 915742노트

반응식

HRID 915742 반응식
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[NH:6][CH:7]=[N:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:21][CH2:22][CH2:23][CH2:24][F:25]>C(#N)C>[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[N:6]([CH2:21][CH2:22][CH2:23][CH2:24][F:25])[CH:7]=[N:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 100221-Bromo-4-fluorobutaneHCID 11430Potassium CarbonateHCID 100362767-Chloro-4H-benzo[e][1,2,4]thiadiazine 1,1-dioxide

생성물 1

HCID 694152107-Chloro-4-(4-fluorobutyl)-4H-1,2,4-benzothiadiazine 1,1-dioxide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
100 °C

실험 절차

150 mg of the compound obtained in Step A of Example 1 are dissolved in 8 ml of acetonitrile, to which 300 mg of K2CO3 and 0.15 ml of 1-bromo-4-fluorobutane are added. The reaction mixture is introduced into a sealed autoclave and is heated at 100° C. for 3 hours. After cooling, the solvent is evaporated off under reduced pressure and the residue is taken up in a minimum of water. The insoluble material is collected by filtration, washed with water and dried. The precipitate is then recrystallised from a minimum of ethyl acetate with the aid of heat. After cooling, the title compound is collected by filtration, washed with a minimum of ethyl acetate and dried.

후처리

  1. additionare added
  2. additionThe reaction mixture is introduced into a sealed autoclave
  3. temperatureAfter cooling
  4. customthe solvent is evaporated off under reduced pressure
  5. filtrationThe insoluble material is collected by filtration
  6. washwashed with water
  7. customdried
  8. customThe precipitate is then recrystallised from a minimum of ethyl acetate with the aid
  9. temperatureof heat
  10. temperatureAfter cooling
  11. filtrationthe title compound is collected by filtration
  12. washwashed with a minimum of ethyl acetate
  13. customdried

출처 및 근거

ORD 기록
ord-d4f40c2eb7f745509f9fcd77489c0491
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268129B2

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