2-Methyl-2-butene → HCID 178454342、化合物

HRID 1875072ノート

反応式

HRID 1875072 の反応式
Cl([O-])=O.[Na+].[OH2:5].P([O-])(O)(O)=O.[Na+].[CH3:12][C:13]([O:16][C:17]([N:19]([C:27]1[NH:28][C:29]([CH:33]=[O:34])=[C:30]([Br:32])[N:31]=1)[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])=[O:18])([CH3:15])[CH3:14].CC(=CC)C>O.C1COCC1.CC(O)(C)C>[CH3:26][C:23]([O:22][C:20]([N:19]([C:17]([O:16][C:13]([CH3:12])([CH3:14])[CH3:15])=[O:18])[C:27]1[NH:28][C:29]([C:33]([OH:5])=[O:34])=[C:30]([Br:32])[N:31]=1)=[O:21])([CH3:24])[CH3:25]

参加物

8

反応物 4

HCID 105532-Methyl-2-buteneHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 23668197Sodium ChloriteHCID 178454341HCID 178454341、化合物

生成物 1

HCID 178454342HCID 178454342、化合物収率 30.1%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of sodium chlorite (0.348 g, 3.84 mmol) and sodium dihydrogenphosphate monohydrate (0.318 g, 2.306 mmol) in water (4 mL) was added to a solution of bis(1,1-dimethylethyl)(4-bromo-5-formyl-1H-imidazol-2-yl)imidodicarbonate (0.150 g, 0.384 mmol), 2-methyl-2-butene (2M in THF) (2.402 mL, 4.80 mmol), t-BuOH (2 mL) and THF (6 mL). The mixture was stirred at RT overnight and extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated. The residue was triturated with ether to give the desired product (0.047 g, 30%) as a white solid. ES MS: m/z 406 (M+1).

後処理

  1. extractionextracted with EtOAc
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was triturated with ether

出典と根拠

ORDレコード
ord-03d9090abadb48d7b2f7f5ab1a5cfd75
出典データセット
uspto-grants-2012_11
特許番号
US08304419B2

反応ノート

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