Phosphorus oxychloride → HCID 57743058、化合物

HRID 1896419ノート

反応式

HRID 1896419 の反応式
[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]

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178432076HCID 178432076、化合物

生成物 1

HCID 57743058HCID 57743058、化合物収率 89%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2fb6e3e00e2647d88d9e055f33730721
出典データセット
uspto-grants-2013_08
特許番号
US08518943B2

反応ノート

読み込み中…