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Potassium Carbonate → HCID 86686286, 화합물

HRID 2172598
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HRID 2172598 반응식
[CH3:1][O:2][C:3](=[O:30])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([N:11]2[C:16](=[O:17])[C:15]([Cl:18])=[C:14]([O:19][CH2:20][C:21]3[CH:26]=[CH:25][C:24](OC)=[CH:23][CH:22]=3)[N:13]=[C:12]2[CH3:29])[CH:5]=1.[F:31]C1C=CC(CBr)=CC=1.C(=O)([O-])[O-].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>CN(C)C=O>[CH3:1][O:2][C:3](=[O:30])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([N:11]2[C:16](=[O:17])[C:15]([Cl:18])=[C:14]([O:19][CH2:20][C:21]3[CH:26]=[CH:25][C:24]([F:31])=[CH:23][CH:22]=3)[N:13]=[C:12]2[CH3:29])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 680214-Fluorobenzyl bromideHCID 86686287HCID 86686287, 화합물

생성물 1

HCID 86686286HCID 86686286, 화합물수율 38%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of Intermediate 3 (120 mg, 0.39 mmol) in N,N-dimethylformamide (2 mL) was added 4-fluorobenzyl bromide (0.05 mL, 0.39 mmol), potassium carbonate (81 mg, 0.58 mmol) and 18-crown-6 (10 mg). The slurry was stirred at ambient temperature for two hours. The reaction was partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulfate. The slurry was filtered and concentrated in vacuo. The crude material was purified using normal phase chromatography (ethyl acetate/heptane) to provide the alkylated product as a colorless oil. (63 mg, 38% yield). MS (M+H): 417

후처리

  1. customThe reaction was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe slurry was filtered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified

출처 및 근거

ORD 기록
ord-78bc2b22c7dc4123aaa8e785412c92bb
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056110B2

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