Sodium Hydroxide → 6-Hydroxy-4,4-dimethylhexane-1,2-diyl dinitrate

HRID 1676005ノート

反応式

HRID 1676005 の反応式
[N+](C1C=CC(C([O:10][CH2:11][CH2:12][C:13]([CH3:26])([CH3:25])[CH2:14][CH:15]([O:21][N+:22]([O-:24])=[O:23])[CH2:16][O:17][N+:18]([O-:20])=[O:19])=O)=CC=1)([O-])=O.[OH-].[Na+]>C1COCC1.CCO.C(=O)(O)[O-].[Na+]>[N+:18]([O-:20])([O:17][CH2:16][CH:15]([O:21][N+:22]([O-:24])=[O:23])[CH2:14][C:13]([CH3:26])([CH3:25])[CH2:12][CH2:11][OH:10])=[O:19]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 582094543,3-Dimethyl-5,6-bis(nitrooxy)hexyl 4-nitrobenzoate

生成物 1

HCID 597787456-Hydroxy-4,4-dimethylhexane-1,2-diyl dinitrate

試薬・触媒・溶媒 2

HCID 516892Sodium Bicarbonate溶媒HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

To a solution of 3,3-dimethyl-5,6-bis(nitrooxy)hexyl 4-nitrobenzoate (1.9 g, 4.73 mmol) in THF:EtOH 1:1 (12 ml) a aqueous solution of NaOH 3N (3.8 ml, 11.4 mmol) was added and the mixture was stirred at room temperature for 3 hrs. Then the mixture was diluted with a saturated solution of sodium bicarbonate and the product was extracted with EtOAc (3×30 ml). The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure, affording the title compound which was used in the subsequent step without further purification.

後処理

  1. extractionthe product was extracted with EtOAc (3×30 ml)
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5a7fb8c7b8e348bba5198b718f1aa3a2
出典データセット
uspto-grants-2011_08
特許番号
US08003811B2

反応ノート

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