Methyl Ethyl Ketone → Methyl 3-methylpent-2-enoate

HRID 1510125ノート

反応式

HRID 1510125 の反応式
C(OP([CH2:9][C:10]([O:12][CH3:13])=[O:11])(OCC)=O)C.C[O-].[Na+].[CH3:17][C:18](=O)[CH2:19][CH3:20]>O>[CH3:13][O:12][C:10](=[O:11])[CH:9]=[C:18]([CH3:17])[CH2:19][CH3:20]

参加物

5

反応物 3

HCID 6569Methyl Ethyl KetoneHCID 66113Methyl diethylphosphonoacetateHCID 10942334Sodium Methoxide

生成物 1

HCID 521288Methyl 3-methylpent-2-enoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 0° C. mixture of methyl diethylphosphonoacetate (12.7 ml, 69.3 mmol) and sodium methoxide (13.0 ml, 69.3 mmol) was added dropwise 2-butanone (5.81 ml, 69.3 mmol) over 30 min. After the addition, the mixture warmed to rt and stirred overnight. To the reaction was added 20 mL of H2O. The mixture was extracted with EtOAc (3 times). The combined organics were dried with MgSO4, filtered, and concentrated. The crude oil was distilled at 110° C. at 35 mmHg to give the desired product.

後処理

  1. additionAfter the addition
  2. extractionThe mixture was extracted with EtOAc (3 times)
  3. dry with materialThe combined organics were dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. distillationThe crude oil was distilled at 110° C. at 35 mmHg

出典と根拠

ORDレコード
ord-8a21c7b5779d480fad1ca79d24454987
出典データセット
uspto-grants-2012_07
特許番号
US08211904B2

反応ノート

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