Water → 3-(Dimethoxymethyl)-4,4-dimethoxybutanenitrile

HRID 1850670ノート

反応式

HRID 1850670 の反応式
[CH3:1][O:2][CH:3]([O:16][CH3:17])[CH:4]([CH:11]([O:14][CH3:15])[O:12][CH3:13])[CH2:5][CH2:6]S([O-])(=O)=O.C(OCC)(=O)C.O.CC#[N:27]>[C-]#N.C([N+](CC)(CC)CC)C>[CH3:1][O:2][CH:3]([O:16][CH3:17])[CH:4]([CH:11]([O:14][CH3:15])[O:12][CH3:13])[CH2:5][C:6]#[N:27]

参加物

6

反応物 4

HCID 962WaterHCID 6342AcetonitrileHCID 8857Ethyl AcetateHCID 86720913[2-(Dimethoxymethyl)-3,3-dimethoxypropyl]methanesulfonate

生成物 1

HCID 867208913-(Dimethoxymethyl)-4,4-dimethoxybutanenitrile

試薬・触媒・溶媒 1

HCID 3014735Tetraethylammonium cyanide触媒

実験手順

Tetraethylammonium cyanide (142.3 g, 910.8 mmol) was added portionwise over 10 minutes to a solution of [2-(dimethoxymethyl)-3,3-dimethoxypropyl]methanesulfonate (124 g, 455.4 mmol) in MeCN (1.24 L). The reaction mixture was stirred at room temperature for 72 h, then portioned between ethyl acetate (1.24 L) and water (1.24 L). The layers were separated and the organic layer was isolated, washed with brine. The organics were dried over MgSO4, filtered and evaporated to give 3-(dimethoxymethyl)-4,4-dimethoxybutanenitrile 11 as a dark brown oil (86.1 g).

後処理

  1. customThe layers were separated
  2. customthe organic layer was isolated
  3. washwashed with brine
  4. dry with materialThe organics were dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-992c14a3fcdc498ca638097f7af61b79
出典データセット
uspto-grants-2015_02
特許番号
US08957078B2

反応ノート

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