Methanol → HCID 57826680, 화합물

HRID 2392088노트

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HRID 2392088 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:10]([OH:12])=[O:11])[S:5][C:6]=1[CH2:7][CH2:8][CH3:9].S(=O)(=O)(O)O.O.[CH3:19]O>>[Br:1][C:2]1[CH:3]=[C:4]([C:10]([O:12][CH3:19])=[O:11])[S:5][C:6]=1[CH2:7][CH2:8][CH3:9]

참가 물질

5

반응물 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 38431344-bromo-5-propylthiophene-2-carboxylic acid

생성물 1

HCID 57826680HCID 57826680, 화합물수율 93%

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온도
50 °C

실험 절차

To a solution of 4-bromo-5-propyl-2-thiophenecarboxylic acid (5.0 g, 20.07 mmol) in methanol (100 ml) was added sulfuric acid (5.35 ml, 100 mmol). The resulting solution stirred at 50° C. for 36 h. H2O (50 mL) was added the aqueous phase was washed several times with DCM. The combined organic fractions were washed with saturated NaHCO3, dried over Na2SO4, concentrated and used directly without further purification providing methyl 4-bromo-5-propyl-2-thiophenecarboxylate (5.1 g, 18.61 mmol, 93% yield) as a yellow oil: LCMS (ES) m/e 262, 264 (M, M+2)+.

후처리

  1. washwas washed several times with DCM
  2. washThe combined organic fractions were washed with saturated NaHCO3
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customused directly without further purification

출처 및 근거

ORD 기록
ord-9ef42163ed95452aa831fcb2aa49a252
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273782B2

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