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Methyl Ethyl Ketone → HCID 21409920, 화합물

HRID 2072006
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HRID 2072006 반응식
[CH3:1][NH:2][C:3]([CH3:7])([CH3:6])[C:4]#[N:5].[CH2:8](Br)[CH:9]=[CH2:10].C(=O)([O-])[O-].[Na+].[Na+].C(C(C)=O)C>CCOCC.[I-].[Na+]>[CH2:10]([CH2:1][NH:2][C:3]([CH3:7])([CH3:6])[C:4]#[N:5])[CH:9]=[CH2:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6569Methyl Ethyl KetoneHCID 7841Allyl bromideHCID 10340Sodium CarbonateHCID 25302512-Methyl-2-(methylamino)propanenitrile

생성물 1

HCID 21409920HCID 21409920, 화합물수율 48.2%

시약·촉매·용매 2

HCID 5238Sodium Iodide촉매HCID 3283Diethyl Ether

실험 절차

A mixture of 2-methylamino-2-methylpropionitrile (14.7 g., 0.15 mole) allyl bromide (18.0g., 0.15 mole), sodium carbonate (15.9 g., 0.15 mole), sodium iodide (0.2 g., 0.001 mole) and methyl ethyl ketone (200 ml.) was heated under reflux for 40 hrs. The sodium carbonate was filtered off and the solvent was removed from the filtrate in vacuo to give a yellow oil, T.L.C. (Silica, ether), three components RF 0.8, 0.4 and 0.0. The oil was passed through a column of silica 40 × 3.5 cm. using ether as an eluent to give 2-allylmethylamino-2-methylpropionitrile (10.0 g., 48%)

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 40 hrs
  3. filtrationThe sodium carbonate was filtered off
  4. customthe solvent was removed from the filtrate in vacuo
  5. customto give a yellow oil, T.L.C

출처 및 근거

ORD 기록
ord-3aec7394054c4d62841d4f0e08ed5e91
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04049663

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