Phosphorus oxychloride → HCID 57743058, 화합물

HRID 1896419노트

반응식

HRID 1896419 반응식
[F:1][C:2]1[C:3]([CH3:18])=[N:4][C:5]2[N:6]([N:9]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:11]=2)[C:7]=1O.O=P(Cl)(Cl)[Cl:21]>ClCCl>[Cl:21][C:7]1[N:6]2[N:9]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:11]=[C:5]2[N:4]=[C:3]([CH3:18])[C:2]=1[F:1]

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178432076HCID 178432076, 화합물

생성물 1

HCID 57743058HCID 57743058, 화합물수율 89%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 6-fluoro-5-methyl-2-phenylpyrazolo[1,5-a]pyrimidin-7-ol x133 (25 mmol, 1 eq, 6.2 g) in POCl3 (150 ml) is heated at 125° C. overnight. After cooling to room temperature, the solution is diluted in dichloromethane and quenched on ice (temperature must be kept under 25° C.). After separation of the organic layer, the aqueous phase is extracted twice with dichloromethane. The cumulated organic layers are dried over MgSO4, filtered, evaporated under reduced pressure and the residue purified by chromatography on silicagel (CH2Cl2) to afford 6.6 g of 7-chloro-6-fluoro-5-methyl-2-phenylpyrazolo[1,5-a]pyrimidine x136.

후처리

  1. customquenched on ice (temperature must be kept under 25° C.)
  2. customAfter separation of the organic layer
  3. extractionthe aqueous phase is extracted twice with dichloromethane
  4. dry with materialThe cumulated organic layers are dried over MgSO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customthe residue purified by chromatography on silicagel (CH2Cl2)

출처 및 근거

ORD 기록
ord-2fb6e3e00e2647d88d9e055f33730721
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518943B2

반응 노트

불러오는 중…