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Methanol → Methyl 4-chloro-2-methyl-3-nitrobenzoate

HRID 1161184
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HRID 1161184 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([CH3:11])[C:3]=1[N+:12]([O-:14])=[O:13].[CH3:15]O.S(Cl)(Cl)=O>>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:15])=[O:7])=[C:4]([CH3:11])[C:3]=1[N+:12]([O-:14])=[O:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 107039094-Chloro-2-methyl-3-nitrobenzoic acid

생성물 1

HCID 10657064Methyl 4-chloro-2-methyl-3-nitrobenzoate

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온도
75 °C

실험 절차

A round bottom flask was charged with 4-chloro-2-methyl-3-nitrobenzoic acid (11.00 g, 0.05102 mol) and methanol (110 mL, 2.7 mol) and thionyl chloride (4.5 mL, 0.061 mol) was added at 0° C. and the reaction heated at 75° C. for 3 hours. The solvent was removed under reduced pressure and the residue dissolved in ethyl acetate (300 mL) and washed with aqueous sodium bicarbonate, water and brine. The organic extracts were dried over sodium sulfate and the solvent removed to recover the esters. MS m/z=230.3 (M+H).

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후처리

  1. additionwas added at 0° C.
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue dissolved in ethyl acetate (300 mL)
  4. washwashed with aqueous sodium bicarbonate, water and brine
  5. dry with materialThe organic extracts were dried over sodium sulfate
  6. customthe solvent removed
  7. customto recover the esters

출처 및 근거

ORD 기록
ord-c02916a712bf4fda96931872554bdf30
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816371B2

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