Sodium Iodide → 2-(5-Chloro-2-fluorophenyl)-4-iodo-5,7-dihydrofuro[3,4-d]pyrimidine

HRID 1354317노트

반응식

HRID 1354317 반응식
Cl[C:2]1[C:3]2[CH2:18][O:17][CH2:16][C:4]=2[N:5]=[C:6]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=2[F:15])[N:7]=1.[Na+].[I-:20]>>[Cl:14][C:12]1[CH:11]=[CH:10][C:9]([F:15])=[C:8]([C:6]2[N:7]=[C:2]([I:20])[C:3]3[CH2:18][O:17][CH2:16][C:4]=3[N:5]=2)[CH:13]=1

참가 물질

3

반응물 2

HCID 5238Sodium IodideHCID 211043384-Chloro-2-(5-chloro-2-fluorophenyl)-5,7-dihydrofuro[3,4-d]pyrimidine

생성물 1

HCID 211043072-(5-Chloro-2-fluorophenyl)-4-iodo-5,7-dihydrofuro[3,4-d]pyrimidine

실험 절차

To a suspension of 4-chloro-2-(5-chloro-2-fluorophenyl)-5,7-dihydrofuro[3,4-d]pyrimidine (78 mg, 0.275 mmol, 1 eq) in 57% H(aq) (2 ml) at rt was added NaI (206 mg, 1.37 mmol, 5 eq). The reaction mixture stirred at rt overnight and then was poured onto ice. The product was extracted with chloroform and the aqueous layer was neutralized with NaHCO3 and extracted further with chloroform. The organic layers were combined washed with brine, dried (MgSO4), filtered and evaporated in vacuo to provide a crude residue of 2-(5-Chloro-2-fluorophenyl)-4-iodo-5,7-dihydrofuro[3,4-d]pyrimidine which was not further purified.

후처리

  1. additionwas poured onto ice
  2. extractionThe product was extracted with chloroform
  3. extractionextracted further with chloroform
  4. washThe organic layers were combined washed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-1a20c0ed09f04bcca0119897fbd080a5
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223766B2

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