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

HRID 524856노트

반응식

HRID 524856 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3014735Tetraethylammonium cyanide촉매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-38aa866f0166481b9bbb06105e9e60d1
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340546B2

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