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Hydrochloric Acid → HCID 57386562, 화합물

HRID 420268
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HRID 420268 반응식
Cl.[NH2:2][C@@H:3]1[C@@H:8]([OH:9])[C@H:7]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([F:20])[CH:12]=2)[CH2:6][S:5](=[O:22])(=[O:21])[CH2:4]1.CC([O-])=O.[Na+].[C:28]([C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][CH:39]=1)[CH:35]=O)([CH3:31])([CH3:30])[CH3:29].[BH3-]C#N.[Na+].Cl.C([O-])([O-])=O.[K+].[K+]>CO.C(Cl)Cl>[C:28]([C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][CH:39]=1)[CH2:35][NH:2][C@@H:3]1[C@@H:8]([OH:9])[C@H:7]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([F:20])[CH:12]=2)[CH2:6][S:5](=[O:22])(=[O:21])[CH2:4]1)([CH3:31])([CH3:29])[CH3:30]
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참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 517045Sodium AcetateHCID 5003444Sodium cyanoborohydrideHCID 101925883-Tert-butylbenzaldehydeHCID 131729360HCID 131729360, 화합물

생성물 1

HCID 57386562
HCID 57386562, 화합물

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

To a solution of (3R*,4S*,5S*)-3-amino-5-(3-fluoro-4-nitro-benzyl)-1,1-dioxo-hexahydro-1lambda*6*-thiopyran-4-ol hydrochloride (0.14 g, 0.39 mmol) in MeOH-CH2Cl2 1:1 (3 mL) was added NaOAc (0.065 g, 0.78 mmol) and 3-tert-butyl-benzaldehyde (0.07 g, 0.43 mmol). The reaction mixture was stirred at 25° C. for 0.5 h before NaBH3CN (0.039 g, 0.59 mmol) was added followed by stirring for 16 h. The reaction mixture was acidified with 1N aq. HCl, stirred for 15 min, basified with K2CO3-solution and extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4 and evaporated. The title compound was obtained after purification by flash-chromatography on silica gel (hexane-CH2Cl2-MeOH 20:20:1 to 1:20:5) as a light yellow foam: TLC (EtOAc) Rf=0.45; HPLC RtA=1.78 min; ESIMS [M+H]+=465; 1H NMR (400 MHz, CDCl3): δ 8.02 (t, 1H), 7.1-7.4 (m, 6H), 4.18 (s, 1H), 3.88 (d, 1H), 3.78 (d, 1H), 3.64 (m, 1H), 3.41 (ddd, 1H), 3.24 (ddd, 1H), 3.12 (dt, 1H), 3.00 (dd, 1H), 2.84, (m, 2H), 2.69 (m, 2H), 2.44 (m, 1H), 1.33 (s, 9H).

후처리

  1. additionwas added
  2. stirringstirred for 15 min
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. customevaporated

출처 및 근거

ORD 기록
ord-175a6f05e00d4d73b710c74cd49283eb
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093406B2

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