Water → 7-Methoxy-2-methylbenzofuran

HRID 636532노트

반응식

HRID 636532 반응식
O[CH2:2][C:3]1[O:4][C:5]2[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[CH:8][C:6]=2[CH:7]=1.C([BH3-])#N.[Na+].C(Cl)(Cl)Cl.O>ClC(Cl)C.[I-].[Zn+2].[I-]>[CH3:13][O:12][C:11]1[C:5]2[O:4][C:3]([CH3:2])=[CH:7][C:6]=2[CH:8]=[CH:9][CH:10]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6212ChloroformHCID 5003444Sodium cyanoborohydrideHCID 11788606(7-Methoxy-1-benzofuran-2-yl)methanol

생성물 1

HCID 112751777-Methoxy-2-methylbenzofuran수율 34.8%

시약·촉매·용매 2

HCID 9883512zinc(II)iodide촉매HCID 63651,1-Dichloroethane용매

실험 절차

A mixture of 2-hydroxymethyl-7-methoxybenzofuran (300 mg), sodium cyanoborohydride (796 mg) and zinc iodide (809 mg) in dichloroethane (10 ml) was stirred for 2 hours at ambient temperature and then refluxed overnight. Chloroform and water were added to the reaction mixture, and the separated organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash chromatography (n-hexane:ethyl acetate=15:1, v/v) to give 7-methoxy-2-methylbenzofuran (95 mg).

후처리

  1. temperaturerefluxed overnight
  2. washthe separated organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was purified by flash chromatography (n-hexane

출처 및 근거

ORD 기록
ord-99fd776611a84181b7ae07d92a263e0e
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194396B1

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