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Ammonia → 1,1-Diethoxy-2-methylprop-1-ene

HRID 1769064
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인쇄 미리보기

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HRID 1769064 반응식
N.[K].[CH2:3]([O:5][CH:6]([O:10][CH2:11][CH3:12])[C:7](=[CH2:9])[CH3:8])[CH3:4]>CCOCC>[CH2:3]([O:5][C:6]([O:10][CH2:11][CH3:12])=[C:7]([CH3:9])[CH3:8])[CH3:4]
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참가 물질

5

반응물 3

HCID 222AmmoniaHCID 5462222PotassiumHCID 11194409Methacrolein diethylacetal

생성물 1

HCID 152051731,1-Diethoxy-2-methylprop-1-ene수율 42.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
-35 °C

실험 절차

To ammonia (500 mL) at -35° C. was added FeCl3 ·6H2O (0.1 g),then potassium metal (24.26 g), and then methacrolein diethylacetal (109 g, 0.756 mol) in ether (150 mL). The mixture was stirred at --35° C. for 3 days, then the ammonia was evaporated, additional ether (100 mL) was added and stirring was continued for another day. The mixture was filtered and the filtrate was distilled at 65° C. and 55 mm Hg to afford 46.05 g of 1,1-diethoxy-2,2-dimethylethylene (Formula V: R3 =R4 =CH3 ; R5 =R6 =OC2H5).

후처리

  1. customthe ammonia was evaporated
  2. additionadditional ether (100 mL) was added
  3. stirringstirring
  4. waitwas continued for another day
  5. filtrationThe mixture was filtered
  6. distillationthe filtrate was distilled at 65° C.

출처 및 근거

ORD 기록
ord-5f610d107f9c4835ad0d0cf6edccd3c6
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05380729

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