Hydrochloric Acid → Methyl cis-2-aminocyclobutane-1-carboxylate hydrochloride

HRID 1662081ノート

反応式

HRID 1662081 の反応式
C(OC([NH:11][C@H:12]1[CH2:15][CH2:14][C@H:13]1[C:16]([O:18][CH3:19])=[O:17])=O)C1C=CC=CC=1.[ClH:20]>[C].[Pd].CO>[ClH:20].[NH2:11][C@H:12]1[CH2:15][CH2:14][C@H:13]1[C:16]([O:18][CH3:19])=[O:17]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 11065277HCID 11065277、化合物

生成物 1

HCID 67429734Methyl cis-2-aminocyclobutane-1-carboxylate hydrochloride

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

To a mixture of methyl rel-(1R,2S)-2-{[(benzyloxy)carbonyl]amino}cyclobutanecarboxylate (1.0 g), methanol (20 ml) and 1 M hydrochloric acid (4.0 ml) was added palladium-carbon (4.0 g) at room temperature, followed by stirring at room temperature for 2 hours under a hydrogen atmosphere. The insolubles in the reaction mixture were separated by filtration through Celite and the filtrate was concentrated under reduced pressure. To the residue were added ethyl acetate and acetonitrile, the solid precipitated was separated by filtration, and the filtrate was concentrated to obtain methyl rel-(1R,2S)-2-aminocyclobutanecarboxylate hydrochloride (0.70 g). Methyl rel-(1R,2S)-2-({N5-[(benzyloxy)carbonyl]-N2-[(1-methyl-1H-indol-2-yl)carbonyl]-L-ornithyl}amino)cyclobutanecarboxylate (0.45 g) was obtained by using methyl rel-(1R,2S)-2-aminocyclobutanecarboxylate hydrochloride (0.31 g) in the same method as for Production Process A1.

後処理

  1. customThe insolubles in the reaction mixture were separated by filtration through Celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the residue were added ethyl acetate and acetonitrile
  4. customthe solid precipitated
  5. customwas separated by filtration
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-ebece6e15c8a4c5386df465b89b0f7ae
出典データセット
uspto-grants-2011_10
特許番号
US08030489B2

反応ノート

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