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Allyltributylstannane → 2-(3-allyl-6-chloropyridin-2-yl)-4-fluoro-1H-indole

HRID 595713
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HRID 595713 반응식
FC(F)(F)S(O[C:7]1[C:8]([C:14]2[NH:15][C:16]3[C:21]([CH:22]=2)=[C:20]([F:23])[CH:19]=[CH:18][CH:17]=3)=[N:9][C:10]([Cl:13])=[CH:11][CH:12]=1)(=O)=O.[CH2:26]([Sn](CCCC)(CCCC)CCCC)[CH:27]=[CH2:28].[Li+].[Cl-]>C1COCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:28]([C:7]1[C:8]([C:14]2[NH:15][C:16]3[C:21]([CH:22]=2)=[C:20]([F:23])[CH:19]=[CH:18][CH:17]=3)=[N:9][C:10]([Cl:13])=[CH:11][CH:12]=1)[CH:27]=[CH2:26]
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6

반응물 3

HCID 90628AllyltributylstannaneHCID 433294Lithium ChlorideHCID 903335466-chloro-2-(4-fluoro-1H-indol-2-yl)pyridin-3-yl trifluoromethanesulfonate

생성물 1

HCID 903339482-(3-allyl-6-chloropyridin-2-yl)-4-fluoro-1H-indole수율 68.4%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물
촉매
HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a mixture of 6-chloro-2-(4-fluoro-1H-indol-2-yl)pyridin-3-yl trifluoromethanesulfonate (2 g, 5.1 mmol), allyltributylstannane (2 g, 6.1 mmol) and anhydrous LiCl (256 mg, 6.1 mmol) in THF (30 mL), Pd(PPh3)4 (588 mg, 0.51 mmol) was added under N2 protection. The reaction mixture was stirred at 60° C. overnight. After it was concentrated in vacuo, the residue was purified by column chromatography (PE:EA=400:1˜100:1) to give the product of 2-(3-allyl-6-chloropyridin-2-yl)-4-fluoro-1H-indole (1 g, yield: 68%). 1H-NMR (CDCl3, 400 MHz) δ 9.72 (s, 1H), 7.57 (d, J=8.0 Hz, 1H), 7.12˜7.24 (m, 3H), 7.02 (s, 1H), 6.77 (t, J=8.0 Hz, 1H), 6.04˜6.12 (m, 1H), 5.25 (d, J=10.0 Hz, 1H), 5.13 (d, J=17.2 Hz, 1H), 3.74 (d, J=6.0 Hz, 2H). MS (M+H)+: 287/289.

후처리

  1. additionwas added under N2 protection
  2. concentrationAfter it was concentrated in vacuo
  3. customthe residue was purified by column chromatography (PE:EA=400:1˜100:1)

출처 및 근거

ORD 기록
ord-e417a7062404406d8dfaeaf6d78ba335
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09243002B2

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