Methyl 1-(methyl{[(phenylmethyl)oxy]carbonyl}amino)cyclopropanecarboxylate → Methyl 1-(methylamino)cyclopropane-1-carboxylate

HRID 1366571ノート

反応式

HRID 1366571 の反応式
[CH3:1][N:2](C(OCC1C=CC=CC=1)=O)[C:3]1([C:6]([O:8][CH3:9])=[O:7])[CH2:5][CH2:4]1>CO>[CH3:1][NH:2][C:3]1([C:6]([O:8][CH3:9])=[O:7])[CH2:5][CH2:4]1

参加物

3

反応物 1

HCID 66936097Methyl 1-(methyl{[(phenylmethyl)oxy]carbonyl}amino)cyclopropanecarboxylate

生成物 1

HCID 13556583Methyl 1-(methylamino)cyclopropane-1-carboxylate収率 45.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl 1-(methyl{[(phenylmethyl)oxy]carbonyl}amino)cyclopropanecarboxylate (assumed 6.8 g, 25.91 mmol, 100% theoretical yield) was dissolved in 30 mL of MeOH, degassed and placed under argon. 10% Pd/C (2.04 g) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon overnight. The contents were then degassed, and the Pd/C was removed by filtration through Celite, washing with MeOH. The filtrate was concentrated in vacuo to provide pure methyl 1-(methylamino)cyclopropanecarboxylate (1.53 g, 45% over two step). LCMS: (M+H)+: 130.1.

後処理

  1. customdegassed
  2. addition10% Pd/C (2.04 g) was added
  3. customthe contents were thoroughly degassed
  4. customballoon overnight
  5. customThe contents were then degassed
  6. customthe Pd/C was removed by filtration through Celite
  7. washwashing with MeOH
  8. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-9748c317dcf1473da7c80fcc3dbf7f04
出典データセット
uspto-grants-2011_02
特許番号
US07893056B2

反応ノート

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