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Iodine → 7-Chloro-2-iodofuro[2,3-c]pyridine

HRID 389428
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HRID 389428 반응식
[Cl:1][C:2]1[N:3]=[CH:4][CH:5]=[C:6]2[CH:10]=[CH:9][O:8][C:7]=12.[Li+].CC([N-]C(C)C)C.[I:19]I>C1COCC1>[Cl:1][C:2]1[N:3]=[CH:4][CH:5]=[C:6]2[CH:10]=[C:9]([I:19])[O:8][C:7]=12
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참가 물질

5

반응물 3

HCID 807IodineHCID 2724682Lithium diisopropylamideHCID 128261077-Chlorofuro[2,3-c]pyridine

생성물 1

HCID 866624077-Chloro-2-iodofuro[2,3-c]pyridine수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

7-Chlorofuro[2,3-c]pyridine (7.60 g, 49.7 mmol) was placed in a three-necked flask fitted with a thermometer and nitrogen inlet and then anhydrous tetrahydrofuran (150 mL) was added. The solution was cooled to −78° C. To this cold solution was added gradually 2 M LDA solution (32.3 mL, 64.6 mmol) by syringe and the resulting mixture was stirred for 2 h at −78° C. Then a solution of iodine (15.1 g, 59.5 mmol) in dry THF (100 mL) was added at −78° C. and the resulting mixture was allowed to warm to RT overnight. The reaction was quenched with aqueous sodium thiosulfate (75 mL) and diluted with ethyl acetate (150 mL). The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (2×75 mL). All organic layers were combined, washed with brine, dried over anhydrous Na2SO4, filtered and evaporated to give 13.7 g (99%) of the title compound as a brown solid. 1H NMR (300 MHz, CDCl3): δ 7.06 (s, 1H), 7.40 (d, J=6.0 Hz, 1 H), 8.17 (d, J=6.0 Hz, 1H).

후처리

  1. customfitted with a thermometer and nitrogen inlet
  2. temperatureto warm to RT overnight
  3. customThe reaction was quenched with aqueous sodium thiosulfate (75 mL)
  4. additiondiluted with ethyl acetate (150 mL)
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted with ethyl acetate (2×75 mL)
  7. washwashed with brine
  8. dry with materialdried over anhydrous Na2SO4
  9. filtrationfiltered
  10. customevaporated

출처 및 근거

ORD 기록
ord-0b04ca8204da446ea395bb72d6e76571
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08378104B2

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