Hexane → Benzoic acid, 4-hydroxy-3-nitro-, methyl ester

HRID 354295

반응식

HRID 354295 반응식
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[CH3:14]CCCCC.[Si](C=[N+]=[N-])(C)(C)C>CO.C1C=CC=CC=1>[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:14])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12]

참가 물질

5

반응물 3

HCID 8058HexaneHCID 120334-Hydroxy-3-nitrobenzoic acidHCID 167693Trimethylsilyldiazomethane

생성물 1

HCID 66835Benzoic acid, 4-hydroxy-3-nitro-, methyl ester수율 79%

시약·촉매·용매 1

HCID 21927730Benzene methanol용매

실험 절차

To a stirred solution of 4-hydroxy-3-nitrobenzoic acid (3.00 g, 0.0164 mol) in MeOH-benzene (1:4, v/v) was added dropwise 2.0 M-n-hexane solution of TMSCHN2 (8.2 mL, 0.0164 mol) at room temp. After the resulting solution was stirred for 4 hr at room temp, the mixture was evaporated off in vacuo. The oily residue was chromatographed on silica-gel with CHCl3 as eluent to afford 4.23 g (79%) methyl 4-hydroxy-3-nitrobenzoate as a pale yellow crystalline material.

후처리

  1. customthe mixture was evaporated off in vacuo
  2. customThe oily residue was chromatographed on silica-gel with CHCl3 as eluent

출처 및 근거

ORD 기록
ord-11476f7213434b268980df5e85cadd8c
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756378B2

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