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Triethylamine → HCID 59603843, 화합물

HRID 2046400
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HRID 2046400 반응식
FC(F)(F)C([O-])=O.FC(F)(F)C([O-])=O.[F:15][C:16]1([F:24])[CH2:21][CH2:20][CH2:19][C@H:18]([NH3+:22])[C@H:17]1[NH3+:23].C(N(CC)CC)C.[O:32](C(OC(C)(C)C)=O)[C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=O>ClCCl>[C:36]([O:35][C:33](=[O:32])[NH:22][C@H:18]1[CH2:19][CH2:20][CH2:21][C:16]([F:24])([F:15])[C@@H:17]1[NH2:23])([CH3:39])([CH3:38])[CH3:37]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonateHCID 86660884HCID 86660884, 화합물

생성물 1

HCID 59603843HCID 59603843, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of (1S,2R)-3,3-difluorocyclohexane-1,2-diaminium bis(trifluoroacetate) (7.5 g, 19.8 mmol) in dichloromethane (100 mL) was added triethylamine (11.1 mL, 79.0 mmol) followed by BOC2O (5.52 mL, 23.8 mmol). The reaction was stirred for 10 hr at ambient temperature. Concentrated, and purified by flash chromatography to afford the title compound. 1H NMR (CDCl3, 500 MHz) 4.76 (br s, 1H); 3.39 (m, 1H); 2.71-2.64 (m, 1H); 2.2-2.1 (m, 2H); 1.7-1.59 (m, 2H); 1.56-1.51 (m, 2H); 1.45 (s, 9H); 1.29-1.21 (m, 2H). 19F NMR (CDCl3, 564 MHz) −100.4-−100.9 (d, 1F); −114.35-−114.87 (d, 1F).

후처리

  1. concentrationConcentrated
  2. custompurified by flash chromatography

출처 및 근거

ORD 기록
ord-f02264c5ad5e4e399827f1b0eadccbc4
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592425B2

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