Methanol → HCID 57826680、化合物

HRID 1961121ノート

反応式

HRID 1961121 の反応式
[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]

参加物

5

反応物 4

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

生成物 1

HCID 57826680HCID 57826680、化合物収率 93%

反応条件

温度
50 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-dcf99f27d9be4edaa57def977f9fd034
出典データセット
uspto-grants-2013_04
特許番号
US08410158B2

反応ノート

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