Stannous chloride dihydrate → HCID 57725359, 화합물

HRID 1987869노트

반응식

HRID 1987869 반응식
[C:1]([O:5][C:6](=[O:23])[C@@H:7]([NH:10][C:11](=[O:22])[C:12]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=1[N+:19]([O-])=O)[CH2:8][CH3:9])([CH3:4])([CH3:3])[CH3:2].O.O.[Sn](Cl)Cl>C(O)C.[OH-].[Na+]>[C:1]([O:5][C:6](=[O:23])[C@@H:7]([NH:10][C:11](=[O:22])[C:12]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=1[NH2:19])[CH2:8][CH3:9])([CH3:2])([CH3:3])[CH3:4]

참가 물질

5

반응물 2

HCID 61436Stannous chloride dihydrateHCID 57725370HCID 57725370, 화합물

생성물 1

HCID 57725359HCID 57725359, 화합물수율 88.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

To a stirred solution of (S)-2-(5-chloro-2-nitro-benzoylamino)-butyric acid-tert-butyl ester (5.72 g,) in ethanol (250 ml) at ambient temperature was added tin(II)chloride bis-hydrate (18.8 g). The mixture was stirred at ambient for 16 hours. The volume was reduced to approximately 50 ml under reduced pressure, and reaction mixture was then diluted with 1M NaOH until the precipitate formed re-dissolved (400 ml). The aqueous was then extracted with diethyl ether (3×100 ml). The organic extracts were combined and washed with brine, dried (MgSO4), and concentrated to give the sub-titled compound as a yellow solid (4.60 g, 88% yield). 1H NMR (400 MHz, CDCl3) δ 7.4 (1H, s), 7.2 (1H, d), 6.6 (2H, m), 5.5 (2H, m), 4.6 (1H, m), 2.0 (1H, m), 1.85 (1H, m), 1.5 (9H, s), 0.95 (3H, t) ppm.

후처리

  1. customThe volume was reduced to approximately 50 ml under reduced pressure, and reaction mixture
  2. customformed
  3. dissolutionre-dissolved (400 ml)
  4. extractionThe aqueous was then extracted with diethyl ether (3×100 ml)
  5. washwashed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-28ef8f4f48c1453b873b2a8e8c4e7932
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07553852B2

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