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

HRID 1662081노트

반응식

HRID 1662081 반응식
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]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 11065277HCID 11065277, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ebece6e15c8a4c5386df465b89b0f7ae
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030489B2

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