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

HRID 869712노트

반응식

HRID 869712 반응식
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

참가 물질

5

반응물 4

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 178468554HCID 178468554, 화합물

생성물 1

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

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-c44cbd0f641f4843b26a7f600cad244f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969376B2

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