Cesium carbonate → HCID 21949732, 화합물

HRID 350842노트

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HRID 350842 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([O:30][Si](C(C)(C)C)(C)C)[CH:25]=1)[CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O.O>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([OH:30])[CH:25]=1)[CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1

참가 물질

4

반응물 2

HCID 10796Cesium carbonateHCID 21949679N-(Benzoxazol-2-yl)-N-3-(4-methoxyphenoxy)propyl-3-tert-butyldimethylsilyloxybenzylamine

생성물 1

HCID 21949732HCID 21949732, 화합물

시약·촉매·용매 1

HCID 21962138N,N-Dimethylformamide--water (1/1)용매

실험 절차

N-(Benzoxazol-2-yl)-N-3-(4-methoxyphenoxy)propyl-3-tert-butyldimethylsilyloxybenzylamine (1.9 g, 3.6 mmol) was dissolved in solvent mixture of N,N-dimethylformamide/H2O (10/1) (5.0 mL). Subsequently, cesium carbonate (1.2 g, 3.6 mmol) was added thereto. The mixture was stirred for 3 hours at room temperature, followed by concentration under reduced pressure. Hydrochloric acid (1.0 mol/L) was added thereto. The resultant mixture was extracted with ethyl acetate, followed by washing the organic layer with brine, drying over anhydrous sodium sulfate, and concentration under reduced pressure. The resultant mixture was subjected to purification by silica gel chromatography (n-hexane/ethyl acetate=5/1), whereby the target compound was obtained (1.3 g, 89%).

후처리

  1. concentrationfollowed by concentration under reduced pressure
  2. additionHydrochloric acid (1.0 mol/L) was added
  3. extractionThe resultant mixture was extracted with ethyl acetate
  4. washby washing the organic layer with brine
  5. dry with materialdrying over anhydrous sodium sulfate, and concentration under reduced pressure
  6. customThe resultant mixture was subjected to purification by silica gel chromatography (n-hexane/ethyl acetate=5/1), whereby the target compound
  7. customwas obtained (1.3 g, 89%)

출처 및 근거

ORD 기록
ord-8ffbd388bea846dbaaa0fd824ab761d0
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183295B2

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