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Ethyl Bromide → HCID 67966666, 화합물

HRID 536198
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HRID 536198 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][O:16][C:17]3[CH:22]=[CH:21][NH:20][C:19](=[O:23])[CH:18]=3)=[CH:11][CH:10]=2)=[CH:4][C:3]=1[C:24]([F:27])([F:26])[F:25].[H-].[Na+].Br[CH2:31][CH3:32]>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][O:16][C:17]3[CH:22]=[CH:21][N:20]([CH2:31][CH3:32])[C:19](=[O:23])[CH:18]=3)=[CH:11][CH:10]=2)=[CH:4][C:3]=1[C:24]([F:27])([F:25])[F:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6332Ethyl BromideHCID 24758Sodium hydrideHCID 67958516HCID 67958516, 화합물

생성물 1

HCID 67966666HCID 67966666, 화합물수율 69.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-{[(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)methyl]oxy}-2(1H)-pyridinone (80 mg, 0.202 mmol) in N,N-dimethylformamide (1 mL) was added Sodium hydride (80 mg, 2.00 mmol). After stirring at rt for 10 min, bromoethane (100 μL, 1.34 mmol) was added. The reaction mixture was warmed to 80° C. and stirred for 1 h, then cooled to rt, quenched by addition of methanol, concentrated. Purification via Biotage-Qs system afforded the title product (59.5 mg) as a white solid. LC-MS (ESI): m/z 424 [M+H]+; 3.76 min (ret time).

후처리

  1. temperatureThe reaction mixture was warmed to 80° C.
  2. stirringstirred for 1 h
  3. temperaturecooled to rt
  4. customquenched by addition of methanol
  5. concentrationconcentrated
  6. customPurification via Biotage-Qs system

출처 및 근거

ORD 기록
ord-6f678a938dd2469780cb8591da060d1f
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859573B2

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