Sodium 1-oxidopyridin-1-ium-2-thiolate → 2-[1-(2,6-Difluorophenyl)ethylthio]pyridine 1-oxide

HRID 1903832노트

반응식

HRID 1903832 반응식
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[CH:4](Cl)[CH3:5].[CH:12]1[CH:13]=[CH:14][N+:15]([O-:19])=[C:16]([S-:18])[CH:17]=1.[Na+]>C(O)C>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[CH:4]([S:18][C:16]1[CH:17]=[CH:12][CH:13]=[CH:14][N+:15]=1[O-:19])[CH3:5]

참가 물질

4

반응물 2

HCID 1569Sodium 1-oxidopyridin-1-ium-2-thiolateHCID 5880552-(1-Chloroethyl)-1,3-difluorobenzene

생성물 1

HCID 133042812-[1-(2,6-Difluorophenyl)ethylthio]pyridine 1-oxide

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
75 °C

실험 절차

2,6-Difluoro-alpha-methylbenzyl chloride (16.6 g, 0.094 mol) is dissolved in ethanol (40 ml) and warmed to 75° C. A 40 percent solution of sodium omadine (38.5 g, 0.103 mol) is added dropwise over a period of 30 minutes maintaining a reaction temperature of 75° C. throughout. Once the addition is complete, the reaction mixture is kept between 75° C. and 80° C. for 2 hours. Thereafter the mixture is quenched in ice-water and crude product is filtered off. After recrystallization with ethyl acetate pure title product (10.65 g, 42.4%) is obtained; Melting Point 158°-160° C.

후처리

  1. temperaturemaintaining a reaction temperature of 75° C. throughout
  2. additionOnce the addition
  3. customThereafter the mixture is quenched in ice-water
  4. filtrationcrude product is filtered off
  5. customAfter recrystallization with ethyl acetate pure title product (10.65 g, 42.4%)
  6. customis obtained

출처 및 근거

ORD 기록
ord-f4934dcd00384e88ac9ff6de521ca032
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04438271

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