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Ethylene Glycol → HCID 86745402, 화합물

HRID 1090480
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HRID 1090480 반응식
[C:1]([CH2:3][CH2:4][O:5][CH:6]([O:8][CH2:9][CH2:10][C:11]#[N:12])[CH3:7])#[N:2].C(#N)C=C.C(O)CO.[OH-].[Li+].COC(C)C#N.[C:29]([CH2:31][CH2:32][O:33][CH:34](O)C)#[N:30]>CO>[C:11]([CH2:10][CH2:9][O:8][CH:6]([O:5][CH2:4][CH2:3][C:1]#[N:2])[CH3:7])#[N:12].[CH3:34][O:33][CH2:32][CH2:31][C:29]#[N:30]
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참가 물질

8

반응물 6

HCID 174Ethylene GlycolHCID 3939Lithium HydroxideHCID 7855Acrylonitrile2회HCID 1418292-MethoxypropanenitrileHCID 13931490HCID 13931490, 화합물2회HCID 19915421HCID 19915421, 화합물

생성물 1

HCID 86745402
HCID 86745402, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
50 °C

실험 절차

As in Example 1, bis(2-cyanoethoxy)ethane was prepared by the addition of 623 g (11.73 moles) of acrylonitrile to 310 g (5.0 moles) of ethylene glycol containing 1.0 g of anhydrous lithium hydroxide at 55°-60° C. over a period of 90 min. The reaction was permitted to stir an additional 2 hr at 50° C. The reaction contents were cooled to 25° C. and 88.0 g (2.75 moles) of methanol was added over a period of 1 hr while maintaining the temperature between 25°-30° C. The mixture was allowed to stir an additional 12 hr at room temperature. Analysis by NMR revealed the crude product mixture to be 79.7 wt % of bis(2-cyanoethoxy)ethane, 17.4 wt % methoxypropionitrile, 1.78 wt % methanol, 0.72 wt % of 2-cyanoethoxyethanol, and 0.33 wt % acrylonitrile.

후처리

  1. customThe reaction contents
  2. temperaturewere cooled to 25° C.
  3. temperaturewhile maintaining the temperature between 25°-30° C
  4. stirringto stir an additional 12 hr at room temperature

출처 및 근거

ORD 기록
ord-26b1c6a0de924aad998b2b0f5590e6c4
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05081305

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