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2-Butanone oxime → 2-(Trimethylsilylmethyloxyimino)butane

HRID 1277607
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HRID 1277607 반응식
[Na].[CH3:2][C:3]([CH2:6][CH3:7])=[N:4][OH:5].[CH3:8][Si:9]([CH3:13])([CH3:12])[CH2:10]Cl>CN(C)C=O>[CH3:8][Si:9]([CH2:13][O:5][N:4]=[C:3]([CH2:6][CH3:7])[CH3:2])([CH3:12])[CH3:10]
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참가 물질

5

반응물 3

HCID 72922-Butanone oximeHCID 75361Silane, (chloromethyl)trimethyl-HCID 5360545Sodium

생성물 1

HCID 543227532-(Trimethylsilylmethyloxyimino)butane수율 70%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To the above obtained dispersion of metallic sodium was added 34.8 g (0.4 mole) of methylethylketoxime and the reaction mixture was heated at 60° to 80° C. for about 180 minutes followed by removal of toluene under reduced pressure to give pasty sodium salt of methylethylketoxime. Then, this sodium salt of methylethylketoxime was dispersed in a mixture of 49.2 g (0.4 mole) of trimethylchloromethylsilane and 100 ml of N,N-dimethylformamide and heated at 70° to 80° C. for 3 hours with agitation. The reaction mixture after completion of the reaction was washed with water to remove sodium chloride formed as the by-product and N,N-dimethylformamide and the residue was extracted with diethyl ether followed by evaporation of the ether to give a crude product which was further distilled under reduced pressure to give 48.4 g of a liquid product boiling at 84° C. under 50 mmHg. This product is referred to as compound S-I hereinafter.

후처리

  1. temperatureheated at 70° to 80° C. for 3 hours with agitation
  2. washThe reaction mixture after completion of the reaction was washed with water
  3. customto remove sodium chloride
  4. customformed as the by-product and N,N-dimethylformamide
  5. extractionthe residue was extracted with diethyl ether
  6. customfollowed by evaporation of the ether
  7. customto give a crude product which
  8. distillationwas further distilled under reduced pressure

출처 및 근거

ORD 기록
ord-22e7e3704c5041a3a14f885a57b508b8
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04278666

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