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Lithium borohydride → 3-Bromo-4-iodobenzenemethanol

HRID 724682
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HRID 724682 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[I:12])[C:5](OC)=[O:6].[BH4-].[Li+]>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][OH:6])[CH:9]=[CH:10][C:11]=1[I:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4148881Lithium borohydrideHCID 17750019Methyl 3-bromo-4-iodobenzoate

생성물 1

HCID 166410803-Bromo-4-iodobenzenemethanol수율 65.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of methyl 3-bromo-4-iodobenzoate (110.0 mg, 0.322 mmol) in tetrahydrofuran (2 mL) was added 2 M lithium tetrahydroborate in tetrahydrofuran (0.161 mL) at room temperature. After stirring for 36 h, the reaction was quenched with sat. ammonium chloride solution, diluted with diethyl ether. The aqueous phase was extract with diethyl ether once. The combined organic solutions were dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified with silica gel chromatography (5% to 20% ethyl acetate/hexane) to give a white solid (66 mg, 65%). 1H NMR (400 MHz, CDCl3): δ 7.82 (d, J=8.2 Hz, 1H), 7.63 (m, 1H), 6.98 (m, 1H), 4.63 (s, 2H). LCMS found for C7H5BrI (M+H−H2O)+: m/z=295, 297.

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후처리

  1. customthe reaction was quenched with sat. ammonium chloride solution
  2. additiondiluted with diethyl ether
  3. extractionThe aqueous phase was extract with diethyl ether once
  4. dry with materialThe combined organic solutions were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified with silica gel chromatography (5% to 20% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-041cc6c6b55646d2bdb3be95c0bea49e
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07141596B2

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