Sodium hydride → HCID 178495763、化合物

HRID 255122

反応式

HRID 255122 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 178495763HCID 178495763、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21974620tetrahydrofuran N,N-dimethylformamide溶媒

実験手順

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)+.

後処理

  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)

出典と根拠

ORDレコード
ord-3cf82a9863b64840a797ee1fa474185d
出典データセット
uspto-grants-2011_01
特許番号
US07875639B2

関連ノート

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