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Ammonium Chloride → HCID 57145839, 화합물

HRID 1078729
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HRID 1078729 반응식
[CH2:1]([N:8]([CH3:12])[C:9](=[O:11])[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([N-]C(C)C)(C)C.[Li+].C(OC([N:28]1[CH2:34][C@H:33]([O:35][Si:36]([C:39]([CH3:42])([CH3:41])[CH3:40])([CH3:38])[CH3:37])[CH2:32][C@H:29]1[CH:30]=[O:31])=O)(C)(C)C.[Cl-].[NH4+]>O1CCCC1.O.C(OCC)(=O)C>[CH2:1]([N:8]([CH3:12])[C:9]([CH2:10][CH:30]([C@@H:29]1[CH2:32][C@@H:33]([O:35][Si:36]([C:39]([CH3:42])([CH3:41])[CH3:40])([CH3:37])[CH3:38])[CH2:34][NH:28]1)[OH:31])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 25517Ammonium ChlorideHCID 2724682Lithium diisopropylamideHCID 4578210N-benzyl-N-methylacetamideHCID 10969557tert-Butyl (2S,4R)-4-((tert-butyldimethylsilyl)oxy)-2-formylpyrrolidine-1-carboxylate

생성물 1

HCID 57145839HCID 57145839, 화합물수율 92%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매4회
HCID 8857Ethyl Acetate용매

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온도
-78 °C

실험 절차

Under a nitrogen atmosphere, a solution of N-benzyl-N-methylacetamide (280 mg, 1.67 mmol) in tetrahydrofuran (1 ml) was dropwise added at -78° C. to a solution comprising a 2.0M lithium diisopropylamide--tetrahydrofuran solution (835 μl, 1.67 mmol) and tetrahydrofuran (15 ml). The mixture was stirred at -78° C. for 10 minutes, and then a solution of (2S,4R)-N-tert-butoxycarbonyl-4-tert-butyldimethylsiloxyprolinal (500 mg, 1.52 mmol) in tetrahydrofuran (1 ml) was dropwise added thereto. The reaction mixture was stirred at the same temperature for 10 minutes. Saturated aqueous ammonium chloride was added to the reaction mixture, and then the reaction mixture was poured into a mixture of ethyl acetate--water. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous sodium sulfate and concentrated in vacuo. The obtained oily residue was subjected to silica gel column chromatography (heptane-ethyl acetate=2:1) to give the title compound (549 mg, yield: 73.6%).

후처리

  1. stirringThe reaction mixture was stirred at the same temperature for 10 minutes
  2. washThe organic layer was washed with saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c8977649666a4e01a1abdd6a25182300
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05550121

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