Phosphorus oxychloride → HCID 18446569, 화합물

HRID 1268841노트

반응식

HRID 1268841 반응식
[I:1][C:2]1[S:10][C:9]2[C:8]([C:11]#[N:12])=[CH:7][NH:6][C:5](=O)[C:4]=2[CH:3]=1.O=P(Cl)(Cl)[Cl:16]>>[Cl:16][C:5]1[C:4]2[CH:3]=[C:2]([I:1])[S:10][C:9]=2[C:8]([C:11]#[N:12])=[CH:7][N:6]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 184465252-Iodo-4-oxo-4,5-dihydro-thieno[3,2-c]pyridine-7-carbonitrile

생성물 1

HCID 18446569HCID 18446569, 화합물

실험 절차

To 2-iodo-4-oxo-4,5-dihydro-thieno[3,2-c]pyridine-7-carbonitrile 25 (7.75 g, 25.6 mmol) was added POCl3 (90 mL). The reaction was stirred under reflux overnight. POCl3 was removed by rotary evaporation followed by suspension of solids in H2O (500 mL) and filtration. The solids were washed with copious amounts of H2O, saturated bicarbonate solution, and washed further with H2O to provide upon drying 7.52 g of 26. 1H NMR (400 MHz, d6-DMSO) δ 8.82 (s, 1H), 8.06 (s, 1H).

후처리

  1. temperatureunder reflux overnight
  2. customPOCl3 was removed by rotary evaporation
  3. additionfollowed by suspension of solids in H2O (500 mL)
  4. filtrationfiltration
  5. washThe solids were washed with copious amounts of H2O, saturated bicarbonate solution
  6. washwashed further with H2O
  7. customto provide
  8. dry with materialupon drying 7.52 g of 26

출처 및 근거

ORD 기록
ord-d48673329def480ab4236aed695bed3e
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199119B2

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