Sodium hydride → HCID 178495763, 화합물

HRID 255122

반응식

HRID 255122 반응식
[Br:1][C:2]1[S:6][C:5]([NH:7][C:8]([C:10]23[CH2:19][CH:14]4[CH2:15][CH:16]([CH2:18][CH:12]([CH2:13]4)[CH2:11]2)[CH2:17]3)=[O:9])=[N:4][CH:3]=1.Br[CH2:21][CH2:22][O:23][CH3:24].[H-].[Na+]>O1CCCC1.CN(C)C=O.O>[Br:1][C:2]1[S:6]/[C:5](=[N:7]\[C:8]([C:10]23[CH2:11][CH:12]4[CH2:18][CH:16]([CH2:15][CH:14]([CH2:13]4)[CH2:19]2)[CH2:17]3)=[O:9])/[N:4]([CH2:21][CH2:22][O:23][CH3:24])[CH:3]=1

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 809722-Bromoethyl methyl etherHCID 49760640N-(5-bromo-1,3-thiazol-2-yl)adamantane-1-carboxamide

생성물 1

HCID 178495763HCID 178495763, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 21974620tetrahydrofuran N,N-dimethylformamide용매

실험 절차

A solution of Example 131A (2.55 g, 7.43 mmol), 1-bromo-2-methoxyethane (0.77 mL, 8.15 mmol) and sodium hydride (60%) (386 mg, 9.66 mmol) in tetrahydrofuran/N,N-dimethylformamide (2:1) (60 mL) was heated at 75° C. for 12 hours. The mixture was cooled to ambient temperature, diluted with water, and extracted with dichloromethane. The organic extract was dried (Na2SO4), filtered and concentrated. Purification by chromatography (silica gel, 100% dichloromethane) afforded the title compound. MS (ESI) m/z 399 (M+H)+.

후처리

  1. extractionextracted with dichloromethane
  2. extractionThe organic extract
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by chromatography (silica gel, 100% dichloromethane)

출처 및 근거

ORD 기록
ord-3cf82a9863b64840a797ee1fa474185d
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875639B2

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