Phosphorus oxychloride → 3-Chloro-2-(4-chloro-2-fluorophenyl)-2,4,6,7-tetrahydro-thiopyrano[4,3-c]pyrazole

HRID 441696노트

반응식

HRID 441696 반응식
O[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[F:14])[N:5]=[C:4]2[CH2:15][CH2:16][S:17][CH2:18][C:3]=12.P(Cl)(Cl)([Cl:21])=O.C([O-])(O)=O.[Na+]>C(Cl)(Cl)Cl>[Cl:21][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[F:14])[N:5]=[C:4]2[CH2:15][CH2:16][S:17][CH2:18][C:3]=12

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 178515244HCID 178515244, 화합물

생성물 1

HCID 214172053-Chloro-2-(4-chloro-2-fluorophenyl)-2,4,6,7-tetrahydro-thiopyrano[4,3-c]pyrazole

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

12.4 Parts of 3-hydroxy-2-(4-chloro-2-fluorophenyl)-2,4,6,7-tetrahydro-thiopyrano[4,3-c]pyrazole was reacted with 6.7 parts of phosphorus oxychloride at 155° C. for 3 hours, the reaction mixture poured into 250 parts of chloroform and 250 parts of saturated aqueous NaHCO3 and stirred for 16 hours. The aqueous portion was extracted with 200 parts of chloroform, the chloroform portions combined and washed twice with 200 parts of water, dried with anhydrous magnesium sulfate, and evaporated under a reduced pressure of 50 to 300 mm Hg. to give 6.0 parts of 3-chloro-2-(4-chloro-2-fluorophenyl)-2,4,6,7-tetrahydro-thiopyrano[4,3-c]pyrazole as a black-brown oil which when contacted with a mixture of ether and pentane changed into a light brown solid, m.p. 97°-99° C.

후처리

  1. extractionThe aqueous portion was extracted with 200 parts of chloroform
  2. washwashed twice with 200 parts of water
  3. dry with materialdried with anhydrous magnesium sulfate
  4. customevaporated under a reduced pressure of 50 to 300 mm Hg

출처 및 근거

ORD 기록
ord-f91e7f90c19647a4945925d6b9fbced1
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042373

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