Ammonium Chloride → (7-Methoxy-1-benzofuran-2-yl)methanol

HRID 636531

반응식

HRID 636531 반응식
C([O:3][C:4]([C:6]1[O:7][C:8]2[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:9]=2[CH:10]=1)=O)C.[BH4-].[Li+].[Cl-].[NH4+]>O1CCCC1>[OH:3][CH2:4][C:6]1[O:7][C:8]2[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:9]=2[CH:10]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 521284Ethyl 7-methoxy-1-benzofuran-2-carboxylateHCID 4148881Lithium borohydride

생성물 1

HCID 11788606(7-Methoxy-1-benzofuran-2-yl)methanol수율 106.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-ethoxycarbonyl-7-methoxybenzofuran (360 mg), lithium borohydride (36 mg) in tetrahydrofuran (4 ml) was stirred at ambient temperature overnight and then for 8 hours at 50° C. Saturated ammonium chloride solution was added to the reaction mixture, and the solution was extracted with ethyl acetate. The extract was washed with saturated ammonium chloride solution and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash chromatography (n-hexane—ethyl acetate) to give 2-hydroxymethyl-7-methoxybenzofuran (310 mg).

후처리

  1. waitfor 8 hours at 50° C
  2. extractionthe solution was extracted with ethyl acetate
  3. washThe extract was washed with saturated ammonium chloride solution and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by flash chromatography (n-hexane—ethyl acetate)

출처 및 근거

ORD 기록
ord-ab28d31b44c34453b0bcce9f953c146e
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194396B1

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