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Triethylamine → tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-{[4-(ethoxycarbonyl)-1,3-thiazol-2-yl]methyl}-1,4-oxazepane-4-carboxylate

HRID 1022710
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HRID 1022710 반응식
Br[CH2:2][C:3](=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[NH2:10][C:11](=[S:35])[CH2:12][C@H:13]1[C@H:19]([C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[C:22]([Cl:27])[CH:21]=2)[O:18][CH2:17][CH2:16][N:15]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:14]1.C(N(CC)CC)C.C(OC(OC(C)(C)C)=O)(OC(C)(C)C)=O.C(=O)([O-])O.[Na+]>CCO>[Cl:27][C:22]1[CH:21]=[C:20]([C@@H:19]2[O:18][CH2:17][CH2:16][N:15]([C:28]([O:30][C:31]([CH3:32])([CH3:33])[CH3:34])=[O:29])[CH2:14][C@H:13]2[CH2:12][C:11]2[S:35][CH:2]=[C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[N:10]=2)[CH:25]=[CH:24][C:23]=1[Cl:26]
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참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 66144Ethyl bromopyruvateHCID 90495Di-tert-butyl dicarbonateHCID 516892Sodium BicarbonateHCID 86663871tert-butyl (6R,7R)-6-(2-amino-2-thioxoethyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

생성물 1

HCID 66975587
tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-{[4-(ethoxycarbonyl)-1,3-thiazol-2-yl]methyl}-1,4-oxazepane-4-carboxylate
수율 101.7%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

Ethyl bromopyruvate (0.070 mL, 0.50 mmol) was added to a solution of tert-butyl (6R,7R)-6-(2-amino-2-thioxoethyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (140 mg, 0.33 mmol) in EtOH (5 mL). The reaction mixture was stirred at 80° C. for 2 hr, triethylamine (0.140 mL, 1.00 mmol) and di-tert-butyl dicarbonate (0.115 mL, 0.50 mmol) were added at room temperature, and the mixture was stirred at room temperature for 5 hr. To the reaction mixture was added aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (173 mg).

후처리

  1. stirringthe mixture was stirred at room temperature for 5 hr
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a618fcce9a1f4c5d9e850331cb546ed3
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

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