Potassium bis(trimethylsilyl)amide → HCID 21963706, 화합물

HRID 2212213노트

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HRID 2212213 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][C:10]([N:12]2[CH2:17][CH2:16][CH2:15][CH:14]([NH:18][C:19]([C:21]3[C:22]([C:27]4[C:32](F)=[CH:31][CH:30]=[CH:29][C:28]=4[Cl:34])=[N:23][O:24][C:25]=3[CH3:26])=[O:20])[CH2:13]2)=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C[Si]([N-][Si](C)(C)C)(C)C.[K+]>CN(C)C=O>[Cl:34][C:28]1[C:27]2[C:22]3[C:21](=[C:25]([CH3:26])[O:24][N:23]=3)[C:19](=[O:20])[N:18]([CH:14]3[CH2:15][CH2:16][CH2:17][N:12]([C:10](=[O:11])[CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)[CH2:13]3)[C:32]=2[CH:31]=[CH:30][CH:29]=1

참가 물질

4

반응물 2

HCID 3251421Potassium bis(trimethylsilyl)amideHCID 21963707HCID 21963707, 화합물

생성물 1

HCID 21963706HCID 21963706, 화합물수율 29%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Dissolve 3-(2-chloro-6-fluoro-phenyl)-5-methyl-isoxazole-4-carboxylic acid[1-(4-phenyl-butyryl)-piperidin-3-yl]-amide (300 mg, 0.62 mmol) in N,N-dimethyl-formamide (4 mL) at ambient temperature under a nitrogen atmosphere. Add a solution of potassium bis(trimethylsilyl)amide (0.5 M in toluene, 1.49 mL, 0.75 mmol) and stir for 20 min. at ambient temperature. Quench with water and follow by adding of solid sodium chloride. Extract with ethyl acetate and wash with water and dry over sodium sulfate. Concentrate and elute over silica gel to give 83 mg (29%) of the desired product. MS(ES): (M+1)+ 464.1, 466.1 m/z.

후처리

  1. customQuench with water
  2. additionby adding of solid sodium chloride
  3. extractionExtract with ethyl acetate
  4. washwash with water
  5. dry with materialdry over sodium sulfate
  6. concentrationConcentrate
  7. washelute over silica gel

출처 및 근거

ORD 기록
ord-d1e9d9eb0f334cb5951cdb5f53084938
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101891B2

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