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TERT-BUTYL TRICHLOROACETATE → tert-Butyl 2-(5-amino-2-(N-(1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborol-6-yl)sulfamoyl)phenyl)acetate

HRID 1256113
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HRID 1256113 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([S:12](=[O:25])(=[O:24])[NH:13][C:14]2[CH:15]=[CH:16][C:17]3[CH2:21][O:20][B:19]([OH:22])[C:18]=3[CH:23]=2)=[C:6]([CH2:8][C:9]([OH:11])=[O:10])[CH:7]=1.ClC(Cl)(Cl)C(O[C:31]([CH3:34])([CH3:33])[CH3:32])=O>C1COCC1.C(Cl)Cl.CCOC(C)=O>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([S:12](=[O:24])(=[O:25])[NH:13][C:14]2[CH:15]=[CH:16][C:17]3[CH2:21][O:20][B:19]([OH:22])[C:18]=3[CH:23]=2)=[C:6]([CH2:8][C:9]([O:11][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:10])[CH:7]=1
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참가 물질

6

반응물 2

HCID 4405255TERT-BUTYL TRICHLOROACETATEHCID 53234452HCID 53234452, 화합물

생성물 1

HCID 68300728tert-Butyl 2-(5-amino-2-(N-(1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborol-6-yl)sulfamoyl)phenyl)acetate

시약·촉매·용매 3

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To the solution of 2-(5-amino-2-(N-(1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborol-6-yl)sulfamoyl)phenyl)acetic acid (2.2 g, 6 mmol) in dry THF (20 ml) under nitrogen, added the solution of tert-butyl 2,2,2-trichloroacetate (4.3 ml, 24 mmol) in dry DCM (10 ml), followed by BF3Et2O (0.1 ml, 0.72 mmol). The reaction was stirred at rt overnight. Quenched the reaction with sodium bicarbonate (sat. in water), diluted with EtOAc, washed with 1N HCl, water and brine, dried over anhydrous sodium sulfate. Concentrated, the result was purified by flash chromatography with EtOAc and hexane. Got 650 mg light yellow solid as product. MS calcd for (C19H23BN2O6S): 418.14. MS found (ESI negative): (M−H)−=417.0. 1H NMR (400 MHz, DMSO-d6) δ (ppm): 9.83 (s, 1H), 7.46 (d, J=8.8 Hz, 1H), 7.40 (d, J=1.6 Hz, 1H), 7.19 (d, J=8 Hz, 1H), 7.09 (dd, J=8 Hz, 1H), 6.39 (d, J=6.8 Hz, 1H), 6.37 (s, 1H), 4.84 (s, 2H), 3.77 (s, 2H), 1.37 (s, 9H).

후처리

  1. customQuenched
  2. customthe reaction with sodium bicarbonate (sat. in water)
  3. washwashed with 1N HCl, water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationConcentrated
  6. customthe result was purified by flash chromatography with EtOAc and hexane

출처 및 근거

ORD 기록
ord-9d00be5d632d4cdda571d8e6305d3b24
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461134B2

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