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Sodium ethoxide → 6-Iodo-2-oxindole

HRID 873485
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HRID 873485 반응식
[CH3:1][CH2:2][O-:3].[Na+].C(C(CC)(C([O-])=O)C([O-])=O)C.Cl[C:17]1[CH:22]=[CH:21][C:20]([I:23])=[CH:19][C:18]=1[N+:24]([O-])=O>CN(C)C(=O)C>[I:23][C:20]1[CH:19]=[C:18]2[C:17]([CH2:1][C:2](=[O:3])[NH:24]2)=[CH:22][CH:21]=1
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참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 69515632,2-DiethylpropanedioateHCID 130920511-Chloro-4-iodo-2-nitrobenzene

생성물 1

HCID 534188196-Iodo-2-oxindole수율 53%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
20 °C

실험 절차

To a jacketed reactor, N,N-dimethylacetamide (DMAc) (120 mL) and sodium ethylate (NaOEt) powder (12.1 g) is charged at 20° C. Diethylmalonate (28.8 g) is added dropwise into the above mixture while keeping internal temperature at around 10° C. After finishing addition, warm up the mixture to 20° C., and continue to stir for another 10 minutes. Then, 2-chloro-5-iodonitrobenzene (17 g) is added in one portion, and heat the mixture to 78° C. and stir for usually at least 2.5 hours until process monitor shows almost complete conversion. The resulting mixture is cooled down to 20° C., and it is quenched by 2 N cold aq. HCl solution (180 mL). The bottom yellow oil was transferred to a jacket reactor with ethanol (92 mL) in it. Then, to the above solution the first portion of SnCl2.2H2O (30 g) powder is added, and the resulting mixture is heated to 70° C. and stirred for 1 hour. The second portion of SnCl2.2H2O (30 g) is added, the mixture is stirred usually at least 0.5 hour until process monitor shows almost complete conversion. Then, heat the resulting mixture to 80° C. and add 36% aq. HCl solution (60 mL) during 0.5 hour. The mixture is stirred for at least 2.5 hours until process monitor shows almost complete conversion. Then, to the mixture water (90 mL) is added and the resulting mixture is cooled down to 20° C. Collect the solid by filtration and wash the solid with water (250 mL) to afford the crude 6-iodo-2-oxindole. Then, it is purified by crystallization with acetic acid (HOAc) (110 mL), and followed by washing with 3 N aq. HCl solution (80 mL) to afford the 6-iodo-2-oxindole in 53% yield and 99% HPLC purity (Rt=7.45 min).

후처리

  1. customat around 10° C
  2. additionaddition
  3. temperatureheat the mixture to 78° C.
  4. stirringstir for usually at least 2.5 hours until process monitor
  5. temperatureThe resulting mixture is cooled down to 20° C.
  6. customit is quenched by 2 N cold aq. HCl solution (180 mL)
  7. customThe bottom yellow oil was transferred to a jacket reactor with ethanol (92 mL) in it
  8. additionThen, to the above solution the first portion of SnCl2.2H2O (30 g) powder is added
  9. temperaturethe resulting mixture is heated to 70° C.
  10. stirringstirred for 1 hour
  11. additionThe second portion of SnCl2.2H2O (30 g) is added
  12. stirringthe mixture is stirred usually at least 0.5 hour until process monitor
  13. temperatureThen, heat the resulting mixture to 80° C.
  14. additionadd 36% aq. HCl solution (60 mL) during 0.5 hour
  15. stirringThe mixture is stirred for at least 2.5 hours until process monitor
  16. additionThen, to the mixture water (90 mL) is added
  17. temperaturethe resulting mixture is cooled down to 20° C
  18. customCollect the solid
  19. filtrationby filtration
  20. washwash the solid with water (250 mL)
  21. customto afford the crude 6-iodo-2-oxindole
  22. customThen, it is purified by crystallization with acetic acid (HOAc) (110 mL)
  23. washby washing with 3 N aq. HCl solution (80 mL)

출처 및 근거

ORD 기록
ord-83968f79b26a487cabd3a27d1342fb43
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975418B2

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