Sodium Carbonate → HCID 54211560, 화합물

HRID 719109

반응식

HRID 719109 반응식
[CH3:1][C:2]([CH3:10])([CH3:9])[CH2:3][C@@H:4]([C:6]([OH:8])=[O:7])[NH2:5].Cl(O)(=O)(=O)=O.C1C=[C:20]2C(C(O)(O)[C:25](=O)[C:19]2=[CH:18]C=1)=O.CCO.C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+]>C(OC(C)(C)C)(=O)C.C(OCC)C.C1(C)C=CC=CC=1.CCOC(C)=O.CO.C(Cl)Cl>[CH3:1][C:2]([CH3:10])([CH3:9])[CH2:3][C@@H:4]([C:6]([O:8][C:19]([CH3:25])([CH3:20])[CH3:18])=[O:7])[NH2:5]

참가 물질

12

반응물 5

HCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 24247Perchloric AcidHCID 194032(2S)-2-Amino-4,4-dimethylpentanoic acidHCID 20476630HCID 20476630, 화합물

생성물 1

HCID 54211560HCID 54211560, 화합물수율 96%

시약·촉매·용매 6

HCID 887Methanol용매HCID 1140Toluene용매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매HCID 10908tert-Butyl acetate용매

실험 절차

4-Methylleucine (500 mg, 3.44 mmol) was suspended in 10 ml t-butyl acetate. Perchloric acid (0.2 ml, 3.49 mmol) was added and the flask was stopped with a septum and stirred over night. Analysis was performed using TLC DCM:MeOH, 9:1; staining with a ninhydrine/EtOH solution). The solution was poured into a flask containing 30 ml EtOAc and 30 ml 5% Na2CO3. The aq-layer turned acidic and 2M NaOH was added until pH was approximately 7. The phases were separated and the aq-phase was washed with 2×30 ml EtOAc. The combined organic phases were washed with brine, dried with Na2SO4 and evaporated. A oil was obtained which was co-evaporated with toluene and then with diethyl ether before being placed under vacuum for two days. Mass 665 mg (96% yield). NMR (CDCl3): 1.0 (s, 9H), 1.5 (s, 9H), 1.65–1.95 (m, 2H), 3.82 (t, 1H).

후처리

  1. additionThe solution was poured into a flask
  2. customThe phases were separated
  3. washthe aq-phase was washed with 2×30 ml EtOAc
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried with Na2SO4
  6. customevaporated
  7. customA oil was obtained which

출처 및 근거

ORD 기록
ord-0448c3b88c404a8db665a533c61a01b8
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132416B2

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