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Triethylamine → HCID 58864454, 화합물

HRID 2355984
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HRID 2355984 반응식
C[Si](I)(C)C.[CH3:6][O:7][C:8](=[O:33])[C@H:9]([NH:22]C(OCC1C=CC=CC=1)=O)[CH2:10][C:11]1[C:20]([Br:21])=[CH:19][C:14]2[NH:15][C:16](=[O:18])[O:17][C:13]=2[CH:12]=1.C(N(CC)CC)C>C(#N)C>[CH3:6][O:7][C:8](=[O:33])[C@H:9]([NH2:22])[CH2:10][C:11]1[C:20]([Br:21])=[CH:19][C:14]2[NH:15][C:16](=[O:18])[O:17][C:13]=2[CH:12]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 85247Trimethylsilyl iodideHCID 25136129HCID 25136129, 화합물

생성물 1

HCID 58864454HCID 58864454, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Trimethylsilyliodide (73 mL, 0.73 mmol) was added to a solution of azotropically dried (R)-2-benzyloxycarbonylamino-3-(5-bromo-2-oxo-2,3-dihydro-benzooxazol-6-yl)-propionic acid methyl ester (146 mg, 0.33 mmol) in acetonitrile (10 mL) at room temperature, and the resulting mixture was stirred at room temperature for 2 h. Triethylamine (0.12 mL) was added and the mixture was stirred at room temperature for 15 min. The solvents were removed in vacuo, and the residue was extracted with ethyl acetate. The combined organics were washed with sodium bicarbonate and brine, dried over sodium sulfate and filtered. Solvents were removed and the residue was used directly in the next step. Mass spec. 315.10 (MH)+.

후처리

  1. stirringthe mixture was stirred at room temperature for 15 min
  2. customThe solvents were removed in vacuo
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe combined organics were washed with sodium bicarbonate and brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customSolvents were removed

출처 및 근거

ORD 기록
ord-3ec7c42dd3904cdc9b10ba7b52123b8e
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754732B2

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