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Ethyl trans-crotonate → Ethyl 2-methylcyclopropanecarboxylate

HRID 2422696
ノート
印刷プレビュー

反応式

HRID 2422696 の反応式
[C:1]([O:6][CH2:7][CH3:8])(=[O:5])/[CH:2]=[CH:3]/[CH3:4].[C:9]([O-])(=O)/C=C/C.CC1CC1C([O-])=O>CS(C)=O>[CH3:4][CH:3]1[CH2:9][CH:2]1[C:1]([O:6][CH2:7][CH3:8])=[O:5]
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 429065Ethyl trans-crotonateHCID 6971246CrotonateHCID 225647062-Methylcyclo-propanecarboxylate

生成物 1

HCID 89405Ethyl 2-methylcyclopropanecarboxylate収率 26.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
17.5 °C

実験手順

To a solution of ethyl trans-crotonate (1.20 kg, 1.31 L, 1.00 equivalent) in DMSO (3.00 L) at ambient temperature is added the above preformed ylide solution over 30 min, while the temperature of the reaction mixture is maintained at about 15-20° C. The progress of the reaction is followed by analysis by gas chromatography (GC, conditions below) until only a small amount of residual crotonate relative to the 2-methylcyclo-propanecarboxylate is observed (about 20-24 h). The reaction mixture is split into two equal (8.5 L) portions for work-up; each portion is treated as follows: Methyl t-butyl ether (MTBE, 6 L) is added, and the biphasic mixture is cooled to 15° C. before the dropwise addition of water (6 L) over about 45 min while maintaining the temperature below 23° C. After the phases are separated, the organic phase is washed twice with 10% brine; and the solvent is gently removed under vacuum (400 mbar, bath temperature 35° C.) to afford the ethyl 2-methylcyclopropanecarboxylate (1.00 kg, 26.8%) containing about 3.3 equivalents of MTBE.

後処理

  1. custom(about 20-24 h)
  2. customThe reaction mixture is split into two equal (8.5 L) portions for work-up
  3. additioneach portion is treated
  4. additionMethyl t-butyl ether (MTBE, 6 L) is added
  5. temperaturethe biphasic mixture is cooled to 15° C. before the dropwise addition of water (6 L) over about 45 min
  6. temperaturewhile maintaining the temperature below 23° C
  7. customAfter the phases are separated
  8. washthe organic phase is washed twice with 10% brine
  9. customand the solvent is gently removed under vacuum (400 mbar, bath temperature 35° C.)

出典と根拠

ORDレコード
ord-ccd510b1eac4436f855ba60f6eca04ab
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960419B2

反応ノート

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