Chloroform → Ethyl 5,7-dichloropyrazolo[1,5-a]pyrimidine-2-carboxylate

HRID 869712ノート

反応式

HRID 869712 の反応式
O[C:2]1[CH:7]=C(O)[N:5]2[N:9]=[C:10]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:11]=[C:4]2[N:3]=1.P(Cl)(Cl)([Cl:19])=O.C(=O)(O)[O-].[Na+].[CH:27]([Cl:30])(Cl)Cl>>[Cl:19][C:2]1[CH:7]=[C:27]([Cl:30])[N:5]2[N:9]=[C:10]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:11]=[C:4]2[N:3]=1

参加物

5

反応物 4

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 178468554HCID 178468554、化合物

生成物 1

HCID 86674517Ethyl 5,7-dichloropyrazolo[1,5-a]pyrimidine-2-carboxylate

実験手順

A suspension of ethyl 5,7-dihydroxypyrazolo[1,5-a]pyrimidine-2-carboxylate (9.59 g, 43.0 mmol) and phosphorous oxychloride (20.0 mL, 215 mmol) was refluxed for 1 hr. After being cooled to ambient temperature, the reaction mixture was poured into saturated sodium bicarbonate and chloroform. The organic layer was separated and aqueous layer was extracted with chloroform. The organic layer was combined and concentrated in vacuo to give ethyl 5,7-dichloropyrazolo[1,5-a]pyrimidine-2-carboxylate. MS (APCI): m/z 260/262 (M+H).

後処理

  1. temperaturewas refluxed for 1 hr
  2. customThe organic layer was separated
  3. extractionaqueous layer was extracted with chloroform
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c44cbd0f641f4843b26a7f600cad244f
出典データセット
uspto-grants-2015_03
特許番号
US08969376B2

反応ノート

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