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Methyl chloroformate → Methyl 4-bromothiophene-3-carboxylate

HRID 41644
ノート
印刷プレビュー

反応式

HRID 41644 の反応式
C([Mg]Cl)(C)C.Br[C:7]1[C:11]([Br:12])=[CH:10][S:9][CH:8]=1.Cl[C:14]([O:16][CH3:17])=[O:15]>C1COCC1>[CH3:17][O:16][C:14]([C:7]1[C:11]([Br:12])=[CH:10][S:9][CH:8]=1)=[O:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6586Methyl chloroformateHCID 184523,4-DibromothiopheneHCID 178418918HCID 178418918、化合物

生成物 1

HCID 13487917Methyl 4-bromothiophene-3-carboxylate収率 54.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
2.5 °C

実験手順

A solution of isopropylmagnesium chloride (1.0 g, 9.7 mmol, 1.2 eq.) in THF (5 mL) was added to a solution of 3,4-dibromo-thiophene (2 g, 8.3 mmol, 1.0 eq.) in THF (15 mL), and stirred for 3 hours while the temperature was maintained at 0-5° C. in an ice/salt bath. Methyl chloroformate (1.6 g, 16.9 mmol, 2 eq.) was added dropwise with stirring. The resulting solution was stirred for an additional 16 hours at room temperature. The reaction was then quenched with water (1 mL). The resulting mixture was concentrated under vacuum, then diluted with EtOAc (50 mL). The resulting mixture was washed 1N HCl (1×100 mL) and saturated aqueous NaCl (2×100). The organic layer was concentrated to provide a crude residue, which was applied onto a silica gel column and eluted with EtOAc/PE (1:50) to yield 4-bromothiophene-3-carboxylic acid methyl ester (1.0 g) as a light yellow solid.

後処理

  1. stirringwith stirring
  2. stirringThe resulting solution was stirred for an additional 16 hours at room temperature
  3. customThe reaction was then quenched with water (1 mL)
  4. concentrationThe resulting mixture was concentrated under vacuum
  5. additiondiluted with EtOAc (50 mL)
  6. washThe resulting mixture was washed 1N HCl (1×100 mL) and saturated aqueous NaCl (2×100)
  7. concentrationThe organic layer was concentrated
  8. customto provide a crude residue, which
  9. washeluted with EtOAc/PE (1:50)

出典と根拠

ORDレコード
ord-c217fb16a7c64c86b4269c269401a79b
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530663B2

反応ノート

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