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Water → HCID 86670470, 화합물

HRID 1911854
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HRID 1911854 반응식
[H-].[Na+].[Si:3]([O:10][C@H:11]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C@H:12]1[CH2:16][CH2:15][C@@H:14]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([C:24](=[O:27])[NH:25][CH3:26])=[CH:20][CH:19]=2)[N:13]1[C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])([C:6]([CH3:9])([CH3:8])[CH3:7])([CH3:5])[CH3:4].Br[CH2:42][C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=1[F:49].O>CN(C=O)C>[Si:3]([O:10][C@H:11]([C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1)[C@H:12]1[CH2:16][CH2:15][C@@H:14]([CH2:17][C:18]2[CH:19]=[CH:20][C:21]([C:24](=[O:27])[N:25]([CH2:42][C:43]3[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=3[F:49])[CH3:26])=[CH:22][CH:23]=2)[N:13]1[C:28]([O:30][C:31]([CH3:33])([CH3:32])[CH3:34])=[O:29])([C:6]([CH3:7])([CH3:8])[CH3:9])([CH3:5])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 67968alpha-Bromo-o-fluorotolueneHCID 86670469HCID 86670469, 화합물

생성물 1

HCID 86670470HCID 86670470, 화합물수율 99.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

NaH (6.1 mg of a 60 wt % dispersion in mineral oil, 0.153 mmol, 1 equivalent) was added to a stirred, room temperature mixture tert-butyl (2R,5S)-2-[(R)-{[tert-butyl(dimethyl)silyl]oxy}(phenyl)methyl]-5-[4-(methylcarbamoyl)benzyl]pyrrolidine-1-carboxylate (80 mg, 0.148 mmol) in DMF (0.74 mL), and the mixture was stirred for 10 minutes. 1-(Bromomethyl)-2-fluorobenzene (0.0281 mg, 0.148 mmol, 1 equivalent) was added and the mixture was stirred overnight. Water was then added and the mixture was partitioned with EtOAc. The aqueous layer was extracted with EtOAc (3×), and the combined organic extracts were washed with brine, dried with Na2SO4, filtered, and concentrated in vacuo. The residue was purified by normal phase flash chromatography using silica gel (0-50% hexanes/ethyl acetate). The product was collected and concentrated in vacuo to afford the title compound (95 mg, 99%). LC-MS=669.2 (M+Na)+.

후처리

  1. stirringthe mixture was stirred overnight
  2. customthe mixture was partitioned with EtOAc
  3. extractionThe aqueous layer was extracted with EtOAc (3×)
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried with Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by normal phase flash chromatography
  9. customThe product was collected
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-19233ad963984d078e357f8113d54d50
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08604038B2

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